WO2023241645A1 - System and method for evaporating sample, and delivery needle assembly for system - Google Patents

System and method for evaporating sample, and delivery needle assembly for system Download PDF

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Publication number
WO2023241645A1
WO2023241645A1 PCT/CN2023/100369 CN2023100369W WO2023241645A1 WO 2023241645 A1 WO2023241645 A1 WO 2023241645A1 CN 2023100369 W CN2023100369 W CN 2023100369W WO 2023241645 A1 WO2023241645 A1 WO 2023241645A1
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WO
WIPO (PCT)
Prior art keywords
channel
container
gas
delivery needle
sample
Prior art date
Application number
PCT/CN2023/100369
Other languages
French (fr)
Chinese (zh)
Inventor
吴洪田
陆艮峰
陈晨
Original Assignee
赛默飞世尔（上海）仪器有限公司
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 赛默飞世尔（上海）仪器有限公司 filed Critical 赛默飞世尔（上海）仪器有限公司
Publication of WO2023241645A1 publication Critical patent/WO2023241645A1/en

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/02—Cleaning by the force of jets or sprays
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B5/00—Cleaning by methods involving the use of air flow or gas flow
    • B08B5/02—Cleaning by the force of jets, e.g. blowing-out cavities
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/34—Purifying; Cleaning
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40—Concentrating samples
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40—Concentrating samples
    • G01N1/4022—Concentrating samples by thermal techniques; Phase changes
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40—Concentrating samples
    • G01N1/4055—Concentrating samples by solubility techniques
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40—Concentrating samples
    • G01N1/4022—Concentrating samples by thermal techniques; Phase changes
    • G01N2001/4027—Concentrating samples by thermal techniques; Phase changes evaporation leaving a concentrated sample
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40—Concentrating samples
    • G01N1/4055—Concentrating samples by solubility techniques
    • G01N2001/4061—Solvent extraction

Definitions

  • the present disclosure relates generally to the technical field of chemical analysis instrumentation, and more particularly to a system and method for evaporating a sample, and also to a delivery needle assembly for use in the system and method.
  • evaporation equipment In industries such as food testing, environmental testing, pharmaceuticals, and biology, evaporation equipment is often used to evaporate samples to obtain concentrated samples.
  • This evaporator can be used in conjunction with other instruments, such as solvent extraction systems.
  • the solvent extraction system uses solvents to extract analytes from solid or semi-solid materials under high temperature and pressure to obtain liquid samples. Then, multiple test tubes or sample containers containing liquid samples are placed in an evaporator and heated to concentrate or dry the sample.
  • samples containing analytes extracted by a solvent extraction system need to be manually placed in an evaporator for concentration. Therefore, the sample preparation process takes a long time, and the sample may be contaminated during the operation.
  • US patent US10124270B2 discloses a delivery needle of a blowing evaporation and drying system.
  • the delivery needle includes a solution introduction tube, a gas introduction tube and a cleaning liquid introduction tube that are set together. From the inside to the outside, they are the solution introduction tube, gas introduction tube and so on.
  • Introduction tube and cleaning fluid introduction tube They are used to deliver solution, gas and cleaning fluid to the container respectively.
  • the present disclosure provides a method for evaporating a sample in a container.
  • the method includes: providing a sample to be evaporated to the container through a delivery needle, the delivery needle including a first channel and a third Two channels, the second channel is located outside the first channel, and the outer wall of the delivery needle forming the second channel has a plurality of holes, and the sample enters the container through the first channel; to the The second channel provides solvent and gas so that the solvent located in the second channel is applied to the inner wall of the container through the hole; and heating the container to evaporate the sample in the container, During said heating, gas is optionally supplied to said container through said first channel.
  • the method according to the present disclosure can realize multiple functions of sample injection, collection of residual samples on the inner wall of the container, and accelerated sample evaporation.
  • solvent and gas By applying solvent and gas to the inner wall of the container, it is possible to collect residual samples on the inner wall of the container, which may be caused by sample splashing when the delivery needle provides the sample to be evaporated to the container.
  • the collection of residual samples on the inner wall of the container avoids sample loss during the preparation process, thereby improving the final sample recovery rate.
  • the step of providing a solvent and a gas further includes: applying compressed gas to the solvent, causing the gas-liquid mixture to pass through the hole to form microdroplets, and the microdroplets At least a portion of is applied to the inner wall of the container.
  • compressed gas the gas and solvent can form tiny droplets, which can evenly adhere to the inner wall of the container. These tiny droplets flow downward along the inner wall of the container, removing residues on the inner wall of the container.
  • the sample is brought back to the liquid sample in the container, so that the residual sample on the inner wall of the container can be collected as completely as possible, avoiding sample defects during the preparation process, and improving the sample recovery rate after final evaporation.
  • the step further includes moving the delivery needle downward to a first position, the first position being lower than the delivery needle when performing the step of providing the solvent and gas.
  • the position of the gas step After the step of moving the delivery needle downward, the step further includes providing gas to the container through the first channel.
  • the delivery needle moves to the first position in preparation for subsequent steps of delivering compressed gas to accelerate evaporation. It can be understood that when the delivery needle provides solvent and gas, the position of the delivery needle is higher than the first position for delivering compressed gas for air blowing. Therefore, the delivery needle has a higher position when applying fluid to the container for residual sample collection, which is beneficial.
  • the first position of the delivery needle for air blowing is relatively low, so that the delivery needle can send the gas closer to the liquid sample to be evaporated in the container.
  • the position is conducive to accelerating the evaporation of the sample.
  • the step of heating the container to evaporate the sample within the container is One step includes closing the second channel while providing gas to the container through the first channel. Sealing the second channel can prevent the gas in the container from flowing back through the second channel.
  • the present disclosure also provides a system for evaporating a sample, including: a sample providing device that provides the sample to a container; a gas providing device that provides gas to the container; a solvent providing device a device that provides a solvent to the container; a heating device configured to heat the sample in the container; and a delivery needle device that includes a delivery needle, the delivery needle device
  • the needle includes a first channel and a second channel, the second channel is located outside the first channel, and an outer wall forming the second channel has a plurality of holes.
  • the delivery needle device is configured to fluidly connect the first channel to the sample providing device, and the first channel is optionally in fluid communication to the gas providing device, and the delivery needle device is configured to fluidly connect the first channel to the sample providing device.
  • the two channels are optionally fluidly connected to the solvent supply device or the gas supply device.
  • the system can realize multiple functions of sample injection, collection of residual samples on the inner wall of the container, and sample evaporation.
  • the transport needle can be used to transport samples, collect residual samples on the inner wall of the container, and can also be used to provide gas to achieve The function of accelerating gas evaporation.
  • the system according to the present disclosure has a high degree of automation, and the sample recovery rate is also significantly improved.
  • the delivery needle device includes a moving mechanism that moves the delivery needle up and down relative to the container.
  • the moving mechanism is configured to move the delivery needle to a first position when the first channel is in fluid communication with the gas supply device, the first position being lower than when the second A channel is optionally located where the delivery needle is when in fluid communication with the solvent provider or the gas provider. It can be understood that when the delivery needle is fluidly connected to the solvent supply device or the gas supply device, the delivery needle is in a higher position. Therefore, the solvent and/or gas applied to the container through the outer wall hole of the second channel of the delivery needle also leaves the delivery needle.
  • the delivery needle With a higher position, it can relatively comprehensively cover the inner wall of the container, making the collection of residual samples on the inner wall of the container more complete.
  • the delivery needle When the delivery needle is located at the lower first position, the delivery needle can send the gas to a position closer to the liquid sample to be evaporated in the container, which is beneficial to accelerating the evaporation of the sample.
  • the system according to the present disclosure has a moving mechanism for delivering the needle.
  • This design allows the system to be adapted to containers of different specifications, and also allows the delivery needle to be located at different heights to achieve different functions such as sample injection, collection of residual samples on the inner wall of the container, and accelerated evaporation through air blowing, thus making the system as a whole It has strong adaptability and compact structure, saving limited operating space in the laboratory.
  • the system includes a switching mechanism, the first channel is fluidly connected to the gas providing device via the sample providing device and the switching mechanism, and the second channel is fluidly connected to the gas providing device via the sample providing device and the switching mechanism.
  • the switching mechanism is fluidly connected to the gas supply device and the solvent supply device respectively, and the switching mechanism has a first switching position, a second switching position and a third switching position. In the first switching position, the first channel is fluidly connected to the gas providing device via the sample providing device; in the second switching position, the second channel bypasses the sample providing device and is directly connected to the gas providing device.
  • the device is fluidly connected; in the third switching position, the second channel bypasses the sample providing device and is directly fluidly connected with the solvent providing device.
  • a switching mechanism is provided in the system to realize fluid communication between the first and second channels of the delivery needle and each supply device, thereby simplifying the arrangement of the fluid supply pipeline of the system.
  • the delivery needle assembly of the present disclosure is compact in design and can be used to support the system to achieve different operations. These operations can include sample/solvent injection, gas delivery to accelerate evaporation, and application towards the inner wall of the container. Adding solvent and gas, these operations support the automatic and continuous fluid delivery during the evaporation process.
  • the hole diameter is between 0.2-0.3mm. This pore size facilitates droplet formation.
  • the outer wall is fixed to the inner wall through a welding portion, and the welding portion makes the third end of the second channel closed.
  • the welded part enables reliable connection and sealing of the two channels.
  • Figure 1 shows a schematic block diagram of a system for evaporating a sample according to a preferred embodiment of the present disclosure.
  • Figure 2 shows a schematic diagram of a delivery needle device fitted to a container according to a preferred embodiment of the present disclosure.
  • Figure 4 shows a cross-sectional view of a longitudinal section of a portion of a delivery needle in accordance with a preferred embodiment of the present disclosure.
  • FIG. 5 shows a cross-sectional view taken along the A-A direction in FIG. 4 .
  • FIG. 6 shows a cross-sectional view taken along the B-B direction in FIG. 4 .
  • Figure 7A shows a schematic diagram of delivering a sample to be evaporated to a container through a delivery needle as shown in Figure 3A.
  • Figure 7B shows a schematic diagram of providing gas to a container through a delivery needle as shown in Figure 3A while the sample is evaporating.
  • Figure 7C shows a schematic diagram of residual sample collection on the inner wall of the container by the delivery needle as shown in Figure 3A.
  • Figure 8B shows an enlarged perspective view of the end of a delivery needle according to another preferred embodiment.
  • Figure 1 shows a schematic block diagram of a system for evaporating a sample according to a preferred embodiment of the present disclosure.
  • the sample that needs to be evaporated is placed in the system with the help of a container.
  • the system is used to heat the container to increase the temperature of the liquid sample in the container, thereby allowing the evaporable components in the sample to escape, thereby concentrating or drying the sample. the goal of.
  • the system can also apply pressure gas to the evaporated sample to accelerate the concentration or drying process.
  • the target chemical to be analyzed ie, the analyte
  • the target chemical to be analyzed must be extracted from the substance so that it can be analyzed and detected, for example, qualitatively or quantitatively, using corresponding detection techniques.
  • this type of extraction can be performed by solid-liquid extraction, which dissolves analytes from solid or semi-solid materials.
  • a solid or semi-solid substance can be any material or matrix containing an analyte, such as pharmaceuticals, soil, or food.
  • the "analyte” in the present invention is a chemical that is separated from a solid or semi-solid substance and can subsequently be used for analytical technology detection (such as qualitative or quantitative), such as active ingredients in pharmaceuticals, pesticides in soil, or chemicals in food. Lipids.
  • sample in the present invention refers to the liquid solvent containing the analyte, which can be sent to the evaporation device for concentration.
  • Samples from solid-liquid extraction For example, products should contain analytes leached from solid or semi-solid materials.
  • the system for evaporating samples mainly includes a sample providing device 30 , a gas providing device 20 , a solvent providing device 10 , a switching mechanism 40 and a delivery needle device 60 .
  • Each providing device 10, 20, 30 is fluidly connected to a delivery needle device 60 through which liquid samples, gases and solvents are delivered into a container 90 placed in the system.
  • FIG. 1 shows by way of example four containers 90 , each container being assigned a delivery needle device 60 .
  • the sample providing device 30 in the system is configured for providing a sample to be evaporated to a container 90 placed within the system.
  • the sample providing device 30 in the system may comprise any type of device capable of providing a sample to a container.
  • the sample providing device 30 includes a storage portion for receiving the sample to be evaporated and a transport mechanism.
  • the sample provided in the sample providing device 30 may be directly prepared in the device 30 and provided to the container 90 by the device 30 , or may be prepared by another independent sample preparation device and then loaded into the sample providing device and then provided to the container 90 .
  • the sample providing device 30 shown in FIG. 1 includes four heated extraction units, each heated extraction unit being connected to a delivery needle device 60 through a control valve 31 . It should be understood that the number of heated extraction units may be more or less, and the number of heated extraction units may be configured to correspond to the number of delivery needle devices 60 .
  • the gas providing device 20 in the system is configured to provide gas to the sample providing device 30 to accelerate extraction by the sample providing device 30 .
  • the gas supply device 20 can also directly supply gas to the container 90 through the delivery needle device 60 without passing through the sample supply device 30 .
  • the sample providing device 30 is arranged between the gas providing device 20 and the container 90 , and the gas can be delivered to the container 90 by the gas providing device 20 through the sample providing device 30 .
  • the gas provided by the gas supply device 20 is usually an inert gas, such as nitrogen.
  • the gas supply device 20 can blow nitrogen into the container 90 , thereby realizing the nitrogen blowing function, thereby speeding up the evaporation of the sample and reducing the evaporation time.
  • the gas supply device 20 provides gas that can be used to accelerate and disperse the liquid to form a spray fluid or mist liquid and apply it to the inner wall of the container 90 to achieve residual samples on the inner wall. collect.
  • the gas supply device 20 is preferably configured to provide gas in a pressure range of 350 to 500 Psi. The surrounding gas will be suitable for the accelerated evaporation of the system and the collection of residual samples from the container.
  • the solvent supply device 10 included in the system is configured to provide solvent to a container 90 disposed within the system, and also to provide solvent to the sample supply device 30 for performing solvent extraction operations on various types of analytes.
  • the switching mechanism 40 in the system is configured to realize flow path selection in different modes, so that solvent and gas are transported to corresponding channels of the delivery needle according to the needs of the operating steps performed by the system (to be described in detail below).
  • the solvent supply device 10 includes a solvent supply pipeline 110
  • the gas supply device 20 includes a gas supply pipeline 120 .
  • the solvent supply pipeline 110 and the gas supply pipeline 120 are respectively fluidly connected to the switching mechanism 40 .
  • the switching mechanism 40 includes an electronic rotary valve (ERV valve).
  • the electronic rotary valve includes at least one inlet end, at least two outlet ends, and a rotary switching valve that selectively communicates with the inlet end and one outlet end.
  • the inlet end is operably connected to the gas supply device 20 and the solvent supply device 10, while one outlet end is connected to the sample supply device 30 and thereby to the first channel of the delivery needle in the delivery needle device, and the other outlet end is connected to the delivery needle.
  • the second channel of the delivery needle in the device is connected.
  • the electronic rotary valve may have one inlet end and eight outlet ends, wherein the four outlet ends are respectively connected to one sample providing device 30 to allow Gas or solvent is selectively delivered to the first channel of the corresponding delivery needle 70 , while the other four outlet ends are respectively connected to the delivery needle device to optionally deliver gas or solvent to the second channel of the corresponding delivery needle 70 .
  • the switching mechanism 40 may include a one-way valve and a control valve, and the solvent supply device 10 and the gas supply device 20 realize supply to the sample through the one-way valves and control valves on their respective individually connected pipelines. Control of the delivery of solvents and gases to the device 30 and container 90 is provided.
  • the gas from the supply device 20 can also directly enter the sample supply device 30 without passing through the switching mechanism 40, and flow through the delivery needle device 60 into the container 90.
  • a bypass line 150 is connected between the switching mechanism 40 and the delivery needle device 60 , and the bypass line 150 does not pass through the sample supply device 30 .
  • the solvent from the solvent supply device 10 will bypass the sample supply device 30 and pass through the bypass line 150 directly to the delivery needle device 60 and enter the container 90 .
  • the delivery needle device 60 in the system is configured to be used with containers 90 of various specifications.
  • the device 60 can hold and move the delivery needle for delivering gas, liquid or gas-liquid mixture to the container.
  • Container 90 may be configured with various capacities, such as 60ml, 100ml, 250ml, etc.
  • the container 90 can be configured to have various shapes, such as a flat-bottom bottle shape with only a container opening 91 on the top as shown in Figure 2, a shape with a large center and two small ends and openings at both ends and upper and lower ends as shown in Figure 7B, where The opening at the lower end is adapted to fit a vial (for example, a 2 ml capacity vial) to receive a small volume of sample collected after evaporation.
  • a vial for example, a 2 ml capacity vial
  • the container and vial can be connected via an adapter.
  • FIG 2 illustrates a preferred embodiment delivery needle device 60 and a container 90 for use with the delivery needle device 60.
  • the delivery needle device 60 mainly includes a delivery needle 70, a moving holder 61, a moving mechanism for moving the delivery needle 70 up and down, a fixed holder 64, and a cover 80. As shown in Figure 2, the mobile retainer 61 is fixed
  • the delivery needle device 60 may move the delivery needle in other ways, such as with a driver attached directly to the delivery needle to move it.
  • the delivery needle device 60 may be attached to the container mouth 91 of the container 90 through at least a portion of the closure 80 , as shown in FIG. 2 , the lower projection of the closure 80 being insertably attached to In the container mouth 91, one end of the delivery needle 70 extends through the container mouth 91 of the container 90 and is inserted into the interior of the container 90 through the through hole in the cover 80, and a plurality of O-rings such as O-rings are provided between the cover 80 and the delivery needle 70. 62 to achieve sealing, the delivery needle 70 is movable relative to the cover 80.
  • the lid 8 should form a sealing fit relative to the container mouth 91 to prevent fluid from escaping.
  • FIG. 4 specifically shows the delivery needle 70 with a double-layer structure.
  • the delivery needle 70 includes a first tube member 75 and a second tube member 76.
  • the second tube member 76 surrounds the first tube member 75.
  • the two tube members 75 and 76 are preferably substantially concentrically arranged.
  • the first channel 71 is formed by the hollow space of the inner first pipe member 75.
  • the second channel 72 is composed of a tubular space between the second pipe member 76 and the first pipe member 75 . In this way, the second channel 72 surrounds the first channel 71, and the two channels 71, 72 are separated by at least one wall.
  • the first channel 71 has a first end that can extend into the container 90 and a second end that is connected to the sample providing device 30, and the second channel 72 has a third end that can extend into the container 90 and The fourth end of the solvent supply device 10 is switchably connected to the gas supply device 20 .
  • the first channel 71 has an opening disposed at a first end, in other words, the first end of the first tube 75 is open.
  • the end surface of the open end of the first tube 75 may be configured as an inclined surface, as shown in FIG. 8A .
  • the end of the first tube 75 may be notched along the longitudinal direction of the tube, as shown in Figure 8B.
  • the first pipe member 75 and the second pipe member 76 are assembled and connected through welding to form an integrated delivery needle.
  • the end of the second pipe member 76 corresponding to the third end of the second channel 72 is fixed to the outer surface of the first pipe member 75 through a welding portion, and the welding portion causes the third end of the second channel 72 to be closed.
  • the delivery needle 70 may also include a retainer 78.
  • the cage 78 is fixedly attached to the first tube 75 and the second tube 76 respectively, so as to maintain the relative position between the two tubes.
  • the retainer 78 includes a ring fixedly attached to the end of the second tube 76 and a plurality of connecting ribs extending from the interior of the ring fixedly attached to the outer surface of the first tube 75 .
  • the cage 78 and the first pipe member 75 and the second pipe member 76 are preferably also fixed by welding.
  • a plurality of holes 77 are provided near the third end of the second channel 72. These holes 77 allow the second channel 72 to communicate with the outside to allow solvent or Gas enters and exits through these holes 77 .
  • the purpose of these holes 77 in the outer wall of the second channel 72 is to allow the fluid to be ejected to collect residual samples on the inner wall of the container 90 to avoid sample damage during the preparation process.
  • the fluid is a gas-liquid mixture formed by a combination of compressed gas and solvent.
  • Part of the gas-liquid mixture will be directly sprayed to the inner wall of the container under the action of gas pressure, and then the liquid will flow down along the inner wall, taking away any residue that may be present on the inner wall;
  • Part of the solvent will be atomized under the action of high-pressure gas, forming micro droplets in the internal space of the container.
  • the micro droplets will adhere to the inner wall and flow down the inner wall.
  • the atomized part of the solvent can supplement the surface of the inner wall that is not covered by the spray application. , allowing the residual samples on the inner wall of the container to be collected more fully.
  • the pressure of compressed gas can usually be controlled in the range of 350-500Psi. This pressure The force range is favorable for adequate removal of residues from the inner walls of the container.
  • the plurality of holes 77 are arranged in a circle around the second channel 72 to form a multi-circle hole group on the outer wall.
  • the plurality of hole groups are spaced apart at a predetermined distance along the longitudinal direction of the outer wall of the second channel 72 .
  • the plurality of holes 77 are arranged to form two circles of hole groups.
  • Each hole group has 12 holes, and the plurality of holes 77 in each hole group are evenly spaced from each other in the circumferential direction of the outer wall.
  • the hole 77 extends in the wall of the tube at 90 degrees relative to the longitudinal axis of the delivery needle 70 .
  • these holes 77 obliquely in the extension direction of the wall of the tube relative to the longitudinal axis of the delivery needle 70 (ie the longitudinal direction of the delivery needle) towards the lower end of the delivery needle 7 shown in Figure 2, so that the holes The radially outer side of 77 is closer to the lower third end than the radial inner side of hole 77, so that the ejected fluid will have a component toward the bottom of container 90.
  • the fluid is applied to the inner wall of container 90, there will be a downward component. It can accelerate the downward flow of fluid along the inner wall of the container 90 and improve the residual sample collection effect.
  • the distribution positions of the holes 77 in the two hole groups are not necessarily aligned along the longitudinal direction of the delivery needle.
  • one of the hole groups in the circle near the third end The radial center lines of the hole 77 and the closest hole 77 in a circle of holes away from the third end are circumferentially offset by an angle ⁇ , for example, ⁇ is 15 degrees.
  • ⁇ is 15 degrees.
  • the number of holes 77 of the delivery needle 70 can be more or less, preferably, each circle of hole groups has between 8 and 16 holes.
  • the aperture d1 of the hole 77 on the second channel 72 of the delivery needle 70 can be set between 0.2-0.3 mm, preferably 0.25 mm.
  • the holes 77 with apertures in this range are conducive to the formation of atomized micro-droplets when spraying in the same shape, thereby enabling the solvent to be applied to the inner wall of the container in two ways: jet flow and atomized micro-droplets at the same time, thereby making the inner wall more covered. comprehensive.
  • the aperture d2 of the opening of the third end of the delivery needle can be set between 0.8-1.2 mm, preferably 1 mm.
  • the distance between the outer wall surface of the first pipe member 75 and the inner wall surface of the second pipe member 76 may be between 0.3-0.5 mm.
  • the delivery needle 70 of the delivery needle device 60 includes a first channel 71 and a second channel 72 located outside the first channel 71 .
  • at least two holder channels 65, 66 are provided in the mobile holder 61.
  • One end of one of the holder channels 65 is connected to the first channel 71 of the delivery needle 70
  • the other end of the holder channel 65 is connected to the sample providing device 30 and is connected to the gas providing device 20 and the solvent via the sample providing device 30 and the switching mechanism 40 Apparatus 10 is provided.
  • One end of the other holder channel 66 is connected to the second channel 72 of the delivery needle 70, and the other end of the channel 66 is connected to the second channel 72 of the delivery needle 70.
  • first channel 71 can be in fluid communication with the sample supply device 30 via the delivery needle device 60, and the first channel 71 can optionally be in fluid communication with the gas supply device 20, and the second channel 72 can optionally be in fluid communication with the solvent supply device.
  • the device 10 or the gas supply device 20 is fluidly connected.
  • the switching mechanism 40 is configured to have at least a first switching position, a second switching position and a third switching position.
  • the first switching position the first channel 71 is fluidly connected to the gas providing device 20 via the sample providing device 30; in the second switching position, the second channel 72 bypasses the sample providing device 30 and is directly connected to the gas providing device through the bypass line 150.
  • 20 is fluidly connected; in the third switching position, the second channel 72 bypasses the sample providing device 30 and is directly fluidly connected to the solvent providing device through the bypass line 150 .
  • the system may further include a shut-off device for the second channel 72, the shut-off device being configured to close the second channel 72 when the first channel 71 is in fluid connection with the sample providing device 30 to avoid gas flow within the container.
  • a shut-off device for the second channel 72, the shut-off device being configured to close the second channel 72 when the first channel 71 is in fluid connection with the sample providing device 30 to avoid gas flow within the container.
  • Two-channel 72 reflux outflow system may be a shut-off valve installed in the holder channel 66 that communicates with the second channel 72 .
  • the sample providing device 30 is arranged upstream of the delivery needle device 60 with a delivery pipeline between the two. Therefore, the sample obtained in the sample providing device 30 can be delivered through the delivery pipeline.
  • the holder channel 65 in the needle device flows into the first channel 71 .
  • the gas in the gas supply device 20 flows into the first channel 71 through the gas supply pipe 120 , the switching mechanism 40 , the sample supply device 30 and the holder channel 65 .
  • the gas from the gas supply device 20 can also directly enter the sample supply device 30 without passing through the switching mechanism 40 , and flow through the holder channel 65 and into the first channel 71 .
  • the gas from the gas supply device 20 or the solvent from the solvent supply device 10 flows through the bypass line 150 through the switching mechanism 40 and is sent to the second channel of the delivery needle through the holder channel 66 in the delivery needle device 60 72 to perform the corresponding steps.
  • the system for sample evaporation also includes a negative pressure application device 50 .
  • the negative pressure applying device 50 is connected to the container 90 to provide negative pressure to the container 90, for example, to evacuate.
  • a negative pressure port connected to the negative pressure applying device 50 may be provided on the cover 80 attached to the container 90, and the negative pressure applying device 50 may be connected through the connection port.
  • the gas escaping from the container 90 can also pass through the negative pressure end Mouth discharge.
  • the system may also include a waste gas recovery device, and the negative pressure port on the cover 80 may be connected to the waste gas recovery device, so that the waste gas can be recovered to avoid pollution of the environment and harm to the human body caused by the escaped gas.
  • an independent exhaust gas port can also be provided on the cover 80 of the container 90 for the discharge of escaped gas.
  • Figure 9 shows a step flow chart of a method for evaporating a sample according to a preferred embodiment of the present disclosure.
  • the preferred method flow shown in Figure 9 includes: step S100 of moving the delivery needle to a position for providing a sample to the container, step S102 of providing a sample to be evaporated to the container through the delivery needle, and moving the delivery needle to a position where the sample is provided to the container.
  • Step S104 of applying solvent and gas to the inner wall of the container step S106 of applying solvent and gas to the inner wall of the container, step S108 of moving the delivery needle to the first position of applying gas, step S110 of evaporating the sample in the container, and by conveying Step S112 of supplying gas from the gas supply device to the container.
  • the sample is in a prepared state at S114.
  • step S110 of evaporating the sample in the container refers to a step in which the system performs at least one means to achieve evaporation, such as evaporation through heating. It should be understood that the process shown in Figure 9 is only exemplary, and not every step in the process is necessary, nor does it necessarily have to be performed in the order of the steps shown in Figure 9 .
  • the step S102 of providing the sample to be evaporated to the container through the delivery needle and the step S110 of evaporating the sample in the container may be started simultaneously. However, in alternative embodiments, step S110 may also be executed for a period of time starting from step S102 but not completely completed, or may be executed after step S102 is completed.
  • the delivery needle may not move but directly perform the step S102 of providing the sample to be evaporated to the container through the delivery needle.
  • step S112 of providing gas from the gas supply device to the container through a delivery needle can be omitted, and only step S110 of evaporating the sample in the container is performed to achieve sample evaporation concentration.
  • step S102 of providing the sample to be evaporated to the container 901 through the delivery needle 70 the system provides the sample to be evaporated from the sample providing device 30 to the container 901 through the first channel 71 located inside the delivery needle 70 .
  • Samples entering container 901 may be obtained instantaneously by solvent extraction of the analytes.
  • part of the gas flowing from the gas supply device 20 into the sample supply device 30 will also be sent into the container 901 together with the sample.
  • excess gas in the container 901 will escape through the exhaust port of the cover 80, and is preferably collected into an exhaust gas recovery device, and the pressure inside the container 901 will be released.
  • the step of moving the delivery needle 70 to a position for providing the sample to the container is optionally performed.
  • the moving mechanism of the delivery needle device 60 moves the delivery needle 70 from the original position to a specific position where sample supply to the container is performed.
  • the original position of the delivery needle 70 is usually a position where the lower end of the delivery needle 70 is close to the cover 80 .
  • the delivery needle as shown in FIG. 7A performs supplying the sample to the container at a lower position, so the delivery needle 70 moves vertically downward.
  • FIG. 7A and Figure 7B show two different specifications of containers 901 and 902.
  • the distance the delivery needle 70 moves downward from the original position is different.
  • the moving distance can be set according to the different heights of containers 901 and 902.
  • Figure 7C schematically shows step S106 of applying solvent and gas to the inner wall of the container.
  • the purpose of applying fluid to the inner wall is to collect as much sample remaining on the inner wall of the container 901 as possible to avoid final sample analysis errors due to sample residue on the inner wall. These sample residues may be splashed onto the inner wall of the container 901 when the sample is fed into the container 901, or may be attached to the inner wall of the container 901 during the lowering of the sample liquid level.
  • the step of applying fluid to the inner wall of the container 901 is performed through the second channel 72 of the delivery needle 70 .
  • step S106 of applying the solvent and gas the solvent is first supplied from the solvent supply device 10 to the second channel 72 of the delivery needle 70 through the bypass line 150 .
  • the solvent does not completely leave the second channel 72 through the holes in the outer wall of the second channel 72 , but is at least partially retained in the second channel 72 or in the pipeline connected to the second channel 72 .
  • the gas supply device 20 provides compressed gas to the second channel 72 through the bypass pipeline 150. The compressed gas will act on the solvent remaining in the pipeline, causing the gas and the solvent to combine to form a gas-liquid mixture and flow out of the second channel 72.
  • holes 77 applied to the inner wall of the container 901.
  • the solvent is sent out toward the second channel 72 of the delivery needle 70 through the bypass line 150 between the switching mechanism 40 and the delivery needle device 60.
  • This part of the solvent It does not pass through the sample providing device 30.
  • Sent to container 901 in this step The solvent in the container does not need to be provided through the sample providing device 30.
  • This design shortens the flow distance that the solvent travels before being applied to the inner wall of the container, thereby reducing the possible impact of resistance in the flow path, so that when the solvent and gas are applied to the inner wall of the container At this time, the force on the solvent is more accurately controlled to achieve better cleaning effect on the inner wall.
  • the shortening of the flow distance also allows the amount of solvent sent into the container 901 in this step to be measured relatively accurately.
  • the step S106 of applying solvent and gas to the inner wall of the container can be repeated multiple times, that is, a small amount of solvent is first provided by the solvent supply device 10 to the second channel 72, and then the gas supply device 20 passes through the bypass line. 150 delivers compressed gas, and performs one injection to the inner wall of the container. Immediately or after a period of time, the solvent supply device 10 provides a small amount of solvent to the second channel 72 and the gas supply device 20 delivers the compressed gas again to perform a second injection. .
  • the number of injections can be determined according to the size of the container and the type of sample.
  • step S104 of moving the delivery needle to a position for applying solvent and gas to the inner wall of the container.
  • the moving mechanism in the delivery needle device 60 moves the delivery needle 70 to a position where solvent and gas are applied to the inner wall of the container, such as the position shown in FIG. 7C, where the delivery needle 70 applies solvent and gas to the inner wall of the container.
  • the location is preferably below or near the necked shoulder of the container.
  • the position where the delivery needle 70 shown in FIG. 7C applies solvent and gas to the inner wall is slightly higher than the position where the delivery needle 70 shown in FIG. 7A provides the sample.
  • the position where the delivery needle 70 applies solvent and gas to the inner wall can be set using a program according to the specifications of the selected container.
  • step S104 may be Omit.
  • step S110 of evaporating the sample in the container can be performed, which can reduce the total time of sample preparation.
  • step S106 of applying solvent and gas to the inner wall of the container is also performed simultaneously with step S110 of evaporating the sample in the container.
  • the aforementioned two steps S102 and S106 and step S110 may also be omitted. This can be done, for example, directly after the operator manually places the container containing the sample to be evaporated into the system.
  • the step S112 of providing the gas from the gas supply device to the container through the delivery needle can be started after the step S102 of providing the sample to be evaporated to the container 901 and the step S106 of applying the solvent and gas to the inner wall of the container.
  • the step S110 of evaporating the sample in the container is in progress.
  • step S112 may be initiated simultaneously with the step of evaporating the sample within the container S110.
  • Step S112 is preferably continued until the sample evaporation is completed, but a period of execution time may also be set to end step S112 before the sample evaporation is completed.
  • the system will stop heating the container. After the inside of the system is fully cooled and the temperature drops to a safe value, the prepared sample can be taken out of the system to obtain the target sample.
  • control device or control method of the system can also be configured to optionally perform the step S102 of providing the sample to be evaporated to the container by its delivery needle, the step S106 of applying solvent and gas to the inner wall of the container, and heating the container to make the inside of the container Any one of the steps in step S110 of sample evaporation is required to satisfy Meet the special needs of sample preparation in some cases.
  • the delivery needle 70 may also include one or more third channels between the first channel 71 and the second channel 72 .
  • the third channel is provided in fluid communication with one or more of the solvent providing device 10, the gas providing device 20, and the sample providing device 30 to perform additional operations.
  • the third channel may be connected to an exhaust gas recovery device or a negative pressure application device, and the application of negative pressure or the recovery of exhaust gas may be implemented through the third channel.

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Abstract

A system and method for evaporating a sample, and a delivery needle (70) assembly for the system. The delivery needle (70) is provided with a first channel (71) and a second channel (72); the second channel (72) is located on the outer side of the first channel (71); a plurality of holes (77) are formed on the outer wall of the delivery needle (70) on which the second channel (72) is formed; a sample can enter a container (90) through the first channel (71); the second channel (72) of the delivery needle (70) can provide a solvent and a gas, so that a solvent located in the second channel (72) is applied to the inner wall of the container (90) by means of the holes (77); in addition, in the process of heating the container to evaporate the sample in the container (90), gas is provided for the container (90) through the first channel (71). According to the system and method for evaporating a sample, sample injection can be automatically performed, evaporation is accelerated, and residual samples on a container wall are collected, thereby avoiding sample loss during sample preparation, and improving the sample recovery rate obtained after final evaporation.

Description

对样品进行蒸发的***和方法以及用于该***的输送针组件Systems and methods for evaporating samples and delivery needle assemblies for the systems 技术领域Technical field
本公开总地涉及化学分析仪器的技术领域，尤其涉及一种对样品进行蒸发的***和方法，并且还涉及用于该***和方法的输送针组件。The present disclosure relates generally to the technical field of chemical analysis instrumentation, and more particularly to a system and method for evaporating a sample, and also to a delivery needle assembly for use in the system and method.
背景技术Background technique
在食品检测、环境检测、制药、生物等行业中常常会使用蒸发设备来对样品进行蒸发处理，以获得浓缩的样品。目前市场上已有能够同时对多件样品分别进行浓缩的仪器，这种蒸发器可以与其他仪器，例如溶剂萃取***，配合使用。溶剂萃取***在高温高压下利用溶剂从固体或半固体物质中萃取分析物以获得液体样品，接着，装着液体样品的多个试管或样品容器被放入蒸发器中加热，使得样品浓缩或干燥。在现有技术中，溶剂萃取***所萃取得到的含有的分析物的样品需要被手动放置到蒸发器进行浓缩，因此，样品制备过程时间长，且操作过程中样品可能受到污染。In industries such as food testing, environmental testing, pharmaceuticals, and biology, evaporation equipment is often used to evaporate samples to obtain concentrated samples. There are currently instruments on the market that can concentrate multiple samples at the same time. This evaporator can be used in conjunction with other instruments, such as solvent extraction systems. The solvent extraction system uses solvents to extract analytes from solid or semi-solid materials under high temperature and pressure to obtain liquid samples. Then, multiple test tubes or sample containers containing liquid samples are placed in an evaporator and heated to concentrate or dry the sample. In the existing technology, samples containing analytes extracted by a solvent extraction system need to be manually placed in an evaporator for concentration. Therefore, the sample preparation process takes a long time, and the sample may be contaminated during the operation.
美国专利US10124270B2公开了一种吹气蒸发和干燥***的输送针，该输送针包括套设在一起的溶液导入管、气体导入管以及清洗液导入管，从内到外依次为溶液导入管、气体导入管和清洗液导入管。它们分别用于向容器中输送溶液、气体和清洗液。US patent US10124270B2 discloses a delivery needle of a blowing evaporation and drying system. The delivery needle includes a solution introduction tube, a gas introduction tube and a cleaning liquid introduction tube that are set together. From the inside to the outside, they are the solution introduction tube, gas introduction tube and so on. Introduction tube and cleaning fluid introduction tube. They are used to deliver solution, gas and cleaning fluid to the container respectively.
尽管现有的蒸发设备已对使用过程中存在的部分问题进行了改进，如何提高分析物的回收率，分析物浓缩效率，以及蒸发设备与前道样品提取装置之间的自动化配合度仍是尚需解决的问题。Although existing evaporation equipment has improved some of the problems existing in the use process, how to improve the recovery rate of analytes, the concentration efficiency of analytes, and the degree of automation between the evaporation equipment and the front sample extraction device are still unclear. Problems to be solved.
发明内容Contents of the invention
为克服现有技术中的不足，本公开提供了一种对容器中样品进行蒸发的方法，该方法包括：通过输送针向所述容器提供待蒸发样品，所述输送针包括第一通道和第二通道，所述第二通道位于所述第一通道的外侧，且所述输送针形成第二通道的外壁具有多个孔，所述样品通过所述第一通道进入所述容器；向所述第二通道提供溶剂和气体，以使位于所述第二通道中的溶剂通过所述孔施加至所述容器的内壁；以及加热所述容器，使所述容器内的样品蒸发， 在进行所述加热的过程中，可选地通过所述第一通道向所述容器提供气体。In order to overcome the deficiencies in the prior art, the present disclosure provides a method for evaporating a sample in a container. The method includes: providing a sample to be evaporated to the container through a delivery needle, the delivery needle including a first channel and a third Two channels, the second channel is located outside the first channel, and the outer wall of the delivery needle forming the second channel has a plurality of holes, and the sample enters the container through the first channel; to the The second channel provides solvent and gas so that the solvent located in the second channel is applied to the inner wall of the container through the hole; and heating the container to evaporate the sample in the container, During said heating, gas is optionally supplied to said container through said first channel.
根据本公开的方法能够实现样品进样、容器内壁残留样品收集和样品加速蒸发多个功能。通过提供溶剂和气体施加到容器内壁能够实现容器内壁的残留样品的收集，这些样品在容器内壁上的残留可能是当输送针向容器提供待蒸发样品时样品飞溅造成的。而容器内壁的残留样品的收集避免了制备过程中样品损失，从而提高了最终的样品回收率。The method according to the present disclosure can realize multiple functions of sample injection, collection of residual samples on the inner wall of the container, and accelerated sample evaporation. By applying solvent and gas to the inner wall of the container, it is possible to collect residual samples on the inner wall of the container, which may be caused by sample splashing when the delivery needle provides the sample to be evaporated to the container. The collection of residual samples on the inner wall of the container avoids sample loss during the preparation process, thereby improving the final sample recovery rate.
在本公开的方法，较佳地，提供溶剂和气体的步骤还依次包括：向所述第二通道提供溶剂；在所述溶剂离开所述第二通道的孔之前向所述第二通道提供气体，使所述气体与所述溶剂结合形成气液混合物并使之通出所述孔。提供溶剂和气体的步骤通过提供气液混合物对容器内壁进行残留样品收集，提高了从内壁收集残留样品的收集效率。In the method of the present disclosure, preferably, the steps of providing a solvent and a gas further include: providing a solvent to the second channel; and providing a gas to the second channel before the solvent leaves the hole of the second channel. , the gas and the solvent are combined to form a gas-liquid mixture and passed through the hole. The step of providing solvent and gas improves the collection efficiency of collecting residual samples from the inner wall of the container by providing a gas-liquid mixture for residual sample collection.
在本公开的方法中，较佳地，提供溶剂和气体步骤还包括：将经压缩的气体施加到所述溶剂，使所述气液混合物通出所述孔后形成微滴，所述微滴的至少一部分被施加到所述容器的内壁上。在经压缩的气体的作用下，气体和溶剂能够形成微小的液滴，这些液滴能够均匀地附着到容器内壁上，这些微小的液滴沿着容器内壁向下流动，将容器内壁上的残留样品带回容器内的液态样品中，从而能够尽可能完整收集容器内壁上的残留样品，避免样品在制备过程中缺损，提高最终蒸发后获得的样品回收率。In the method of the present disclosure, preferably, the step of providing a solvent and a gas further includes: applying compressed gas to the solvent, causing the gas-liquid mixture to pass through the hole to form microdroplets, and the microdroplets At least a portion of is applied to the inner wall of the container. Under the action of compressed gas, the gas and solvent can form tiny droplets, which can evenly adhere to the inner wall of the container. These tiny droplets flow downward along the inner wall of the container, removing residues on the inner wall of the container. The sample is brought back to the liquid sample in the container, so that the residual sample on the inner wall of the container can be collected as completely as possible, avoiding sample defects during the preparation process, and improving the sample recovery rate after final evaporation.
在本公开的方法中，较佳地，提供溶剂和气体步骤后还包括将所述输送针向下移动到第一位置，所述第一位置低于所述输送针在执行提供所述溶剂和气体步骤时所处位置。输送针向下移动步骤后还包括通过所述第一通道向所述容器提供气体。输送针移动到第一位置以备后续执行输送压缩气体以加速蒸发的步骤。可以理解，输送针提供溶剂和气体时输送针的位置相对输送压缩气体进行气吹的第一位置更高，因此，通过输送针向容器内施加流体进行残留样品收集时具有较高位置，这有助于相对全面地覆盖容器内壁，使得对容器内壁残留样品的收集更为完整输送针进行气吹的第一位置相对较低，这样输送针能够将气体送到较为靠近容器内待蒸发液态样品的位置，有利于加速样品的蒸发。In the method of the present disclosure, preferably, after the step of providing the solvent and gas, the step further includes moving the delivery needle downward to a first position, the first position being lower than the delivery needle when performing the step of providing the solvent and gas. The position of the gas step. After the step of moving the delivery needle downward, the step further includes providing gas to the container through the first channel. The delivery needle moves to the first position in preparation for subsequent steps of delivering compressed gas to accelerate evaporation. It can be understood that when the delivery needle provides solvent and gas, the position of the delivery needle is higher than the first position for delivering compressed gas for air blowing. Therefore, the delivery needle has a higher position when applying fluid to the container for residual sample collection, which is beneficial. Helps to relatively comprehensively cover the inner wall of the container, making the collection of residual samples on the inner wall of the container more complete. The first position of the delivery needle for air blowing is relatively low, so that the delivery needle can send the gas closer to the liquid sample to be evaporated in the container. The position is conducive to accelerating the evaporation of the sample.
较佳地，所述加热容器使容器内的样品蒸发的步骤与所述通过第一通道向容器提供待蒸发样品的步骤同时开始执行，从而能够节省总的样品制备时间。Preferably, the step of heating the container to evaporate the sample in the container is performed simultaneously with the step of providing the sample to be evaporated to the container through the first channel, thereby saving the total sample preparation time.
本公开的另一个方面，加热所述容器使所述容器内的样品蒸发的步骤进 一步包括：当通过所述第一通道向所述容器提供气体时，封闭所述第二通道。封闭第二通道，可以避免容器内的气体通过第二通道反流。In another aspect of the present disclosure, the step of heating the container to evaporate the sample within the container is One step includes closing the second channel while providing gas to the container through the first channel. Sealing the second channel can prevent the gas in the container from flowing back through the second channel.
本公开还提供了一种对样品进行蒸发的***，包括：样品提供装置，所述样品提供装置向容器提供所述样品；气体提供装置，所述气体提供装置向所述容器提供气体；溶剂提供装置，所述溶剂提供装置向所述容器提供溶剂；加热装置，所述加热装置构造成加热所述容器中的所述样品；以及输送针装置，所述输送针装置包括输送针，所述输送针包括第一通道和第二通道，所述第二通道位于所述第一通道的外侧，形成所述第二通道的外壁具有多个孔。输送针装置构造成使所述第一通道与所述样品提供装置流体相连，且所述第一通道可选地与所述气体提供装置流体相连，并且所述输送针装置构造成使所述第二通道可选地与所述溶剂提供装置或所述气体提供装置流体相连。The present disclosure also provides a system for evaporating a sample, including: a sample providing device that provides the sample to a container; a gas providing device that provides gas to the container; a solvent providing device a device that provides a solvent to the container; a heating device configured to heat the sample in the container; and a delivery needle device that includes a delivery needle, the delivery needle device The needle includes a first channel and a second channel, the second channel is located outside the first channel, and an outer wall forming the second channel has a plurality of holes. The delivery needle device is configured to fluidly connect the first channel to the sample providing device, and the first channel is optionally in fluid communication to the gas providing device, and the delivery needle device is configured to fluidly connect the first channel to the sample providing device. The two channels are optionally fluidly connected to the solvent supply device or the gas supply device.
根据本公开***能够实现样品进样、容器内壁残留样品收集和样品蒸发多个功能，输送针既能用于输送样品，又能够用于容器内壁的残留样品收集，并且也可用于提供气体以实现气体加速蒸发的功能。根据本公开的***自动化程度高，并且样品回收率也有显著提高。According to the disclosed system, the system can realize multiple functions of sample injection, collection of residual samples on the inner wall of the container, and sample evaporation. The transport needle can be used to transport samples, collect residual samples on the inner wall of the container, and can also be used to provide gas to achieve The function of accelerating gas evaporation. The system according to the present disclosure has a high degree of automation, and the sample recovery rate is also significantly improved.
在本公开的***中，输送针装置包括使所述输送针相对所述容器上下移动的移动机构。较佳地，所述移动机构构造成在所述第一通道与所述气体提供装置流体相连的情况下使所述输送针移动到第一位置，所述第一位置低于当所述第二通道可选地与所述溶剂提供装置或所述气体提供装置流体相连时所述输送针所处位置。可以理解，输送针与溶剂提供装置或气体提供装置流体相连时，输送针的位置较高，因此，通过输送针第二通道外壁孔向容器内施加的溶剂和/或气体在离开输送针时也具有较高位置，从而更能够相对全面地覆盖容器内壁，使得针对容器内壁残留样品的收集更为完整。而在输送针位于较低的第一位置时，输送针能够将气体送到较为靠近容器内待蒸发液态样品的位置，有利于加速样品的蒸发。In the system of the present disclosure, the delivery needle device includes a moving mechanism that moves the delivery needle up and down relative to the container. Preferably, the moving mechanism is configured to move the delivery needle to a first position when the first channel is in fluid communication with the gas supply device, the first position being lower than when the second A channel is optionally located where the delivery needle is when in fluid communication with the solvent provider or the gas provider. It can be understood that when the delivery needle is fluidly connected to the solvent supply device or the gas supply device, the delivery needle is in a higher position. Therefore, the solvent and/or gas applied to the container through the outer wall hole of the second channel of the delivery needle also leaves the delivery needle. With a higher position, it can relatively comprehensively cover the inner wall of the container, making the collection of residual samples on the inner wall of the container more complete. When the delivery needle is located at the lower first position, the delivery needle can send the gas to a position closer to the liquid sample to be evaporated in the container, which is beneficial to accelerating the evaporation of the sample.
根据本公开的***由于具有用于输送针的移动机构。这一设计可以使得***能够适配于不同规格的容器使用，也可以使得通过允许输送针位于不同高度来实现进样、容器内壁残留样品收集及通过气吹加速蒸发等不同功能，从而使得***整体适配性强，且结构紧凑，节省实验室内有限的操作空间。The system according to the present disclosure has a moving mechanism for delivering the needle. This design allows the system to be adapted to containers of different specifications, and also allows the delivery needle to be located at different heights to achieve different functions such as sample injection, collection of residual samples on the inner wall of the container, and accelerated evaporation through air blowing, thus making the system as a whole It has strong adaptability and compact structure, saving limited operating space in the laboratory.
在本公开的***中，较佳地，输送针装置包括封盖，所述第一通道和所述第二通道密封地穿过所述封盖，所述封盖构造成密封地配合到容器的容器 口，且所述输送针相对所述封盖可移动。In the system of the present disclosure, preferably, the delivery needle device includes a closure, the first channel and the second channel sealingly passing through the closure, the closure being configured to sealingly fit to the container. container port, and the delivery needle is movable relative to the cover.
在本公开的***中，较佳地，所述***进一步包括负压施加装置和/或废气回收装置。封盖设有连接到所述负压施加装置和/或所述废气回收装置的端口。In the system of the present disclosure, preferably, the system further includes a negative pressure application device and/or an exhaust gas recovery device. The cover is provided with a port connected to the negative pressure applying device and/or the exhaust gas recovery device.
在本公开的***中，较佳地，所述***包括切换机构，所述第一通道经由所述样品提供装置和所述切换机构流体连接到所述气体提供装置，所述第二通道经由所述切换机构与所述气体提供装置和所述溶剂提供装置流体分别相连，所述切换机构具有第一切换位置、第二切换位置和第三切换位置。在第一切换位置，所述第一通道经由所述样品提供装置与所述气体提供装置流体相连；在第二切换位置，所述第二通道绕开所述样品提供装置直接与所述气体提供装置流体相连；在第三切换位置，所述第二通道绕开所述样品提供装置直接与所述溶剂提供装置流体相连。在***中设置切换机构来实现输送针的第一和第二通道与各提供装置的流体连通，简化了***的流体供应管路布置。In the system of the present disclosure, preferably, the system includes a switching mechanism, the first channel is fluidly connected to the gas providing device via the sample providing device and the switching mechanism, and the second channel is fluidly connected to the gas providing device via the sample providing device and the switching mechanism. The switching mechanism is fluidly connected to the gas supply device and the solvent supply device respectively, and the switching mechanism has a first switching position, a second switching position and a third switching position. In the first switching position, the first channel is fluidly connected to the gas providing device via the sample providing device; in the second switching position, the second channel bypasses the sample providing device and is directly connected to the gas providing device. The device is fluidly connected; in the third switching position, the second channel bypasses the sample providing device and is directly fluidly connected with the solvent providing device. A switching mechanism is provided in the system to realize fluid communication between the first and second channels of the delivery needle and each supply device, thereby simplifying the arrangement of the fluid supply pipeline of the system.
在本公开的***中，较佳地，***包括用于所述第二通道的切断装置，所述切断装置构造成当所述第一通道与所述样品提供装置流体相连时封闭所述第二通道。通过切断装置可以在向输送针的第一通道提供气体时封闭第二通道，从而避免容器内的气体通过第二通道反流。In the system of the present disclosure, preferably, the system includes a shut-off device for the second channel, the shut-off device being configured to seal the second channel when the first channel is in fluid communication with the sample providing device. aisle. The shut-off device can close the second channel when gas is supplied to the first channel of the delivery needle, thereby preventing the gas in the container from flowing back through the second channel.
在本公开的***中，较佳地，所述气体提供装置设置成以350-500Psi的压力向所述容器提供气体。In the system of the present disclosure, preferably, the gas supply device is configured to provide gas to the container at a pressure of 350-500 Psi.
在本公开的***中，较佳地，所述输送针还包括第三通道，所述第三通道介于所述第一通道和所述第二通道之间。该第三通道可选地与所述溶剂提供装置或所述气体提供装置流体相连。In the system of the present disclosure, preferably, the delivery needle further includes a third channel, and the third channel is between the first channel and the second channel. The third channel is optionally in fluid communication with the solvent provider or the gas provider.
此外，本公开还提供了一种用于蒸发***的输送针组件，包括：第一通道，所述第一通道具有第一端和第二端；第二通道，所述第二通道具有第三端和第四端，所述第二通道位于所述第一通道的外侧；以及封盖，所述第一通道和所述第二通道密封地穿过所述封盖，所述封盖构造成密封地配合到容器的容器口；其中，所述第一通道具有设置在所述第一端的开口；所述第二通道的所述第三端封闭，形成所述第二通道的外壁具有多个孔，这些孔使得通出第二通道的气液混合物被雾化为微液滴并被施加到容器的内壁。In addition, the present disclosure also provides a delivery needle assembly for an evaporation system, including: a first channel having a first end and a second end; a second channel having a third end and a fourth end, the second channel is located outside the first channel; and a cover, the first channel and the second channel sealingly pass through the cover, the cover is configured to Sealingly fitted to the container mouth of the container; wherein the first channel has an opening provided at the first end; the third end of the second channel is closed, and the outer wall forming the second channel has multiple holes, these holes allow the gas-liquid mixture passing through the second channel to be atomized into micro droplets and applied to the inner wall of the container.
本公开的输送针组件设计紧凑，且可以用于支持***实现不同操作，这些操作可以包括样品/溶剂进样、用于加速蒸发的气体输送、向容器内壁方向施 加溶剂、气体，这些操作支持了蒸发过程中的流体输送能够自动连续地进行。The delivery needle assembly of the present disclosure is compact in design and can be used to support the system to achieve different operations. These operations can include sample/solvent injection, gas delivery to accelerate evaporation, and application towards the inner wall of the container. Adding solvent and gas, these operations support the automatic and continuous fluid delivery during the evaporation process.
根据本公开的输送针组件其第二通道的外壁设有孔，因此，在蒸发加热进行之前或根据设定对容器壁进行喷射清洗，收集容器内壁上的样品残留，避免样品在制备过程中缺损。外壁中的成圈的孔确保了容器内壁上残留的样品能被更充分地收集。According to the delivery needle assembly of the present disclosure, the outer wall of the second channel is provided with a hole. Therefore, before the evaporation and heating is performed or according to the setting, the container wall is spray-cleaned to collect the sample residue on the inner wall of the container to avoid sample damage during the preparation process. . The circle of holes in the outer wall ensures that any remaining sample on the inner wall of the container can be more fully collected.
在本公开的输送针组件中，较佳地，所述第二通道围绕所述第一通道，所述第二通道与所述第一通道通过至少一内壁隔开，其中所述外壁和所述内壁固定为一体。输送针由于具有第一通道和围绕第一通道的第二通道，仅通过一根输送针便能实现进样、容器内壁残留样品收集及输送压力气体加速蒸发等多重功能，简化了管路结构，且便于***的制造和安装。在本公开的输送针组件中，较佳地，所述多个孔靠近所述第二通道的所述第三端设置。In the delivery needle assembly of the present disclosure, preferably, the second channel surrounds the first channel, and the second channel is separated from the first channel by at least one inner wall, wherein the outer wall and the The inner wall is fixed as one. Since the delivery needle has a first channel and a second channel surrounding the first channel, multiple functions such as sample injection, collection of residual samples on the inner wall of the container, and delivery of pressurized gas to accelerate evaporation can be achieved with only one delivery needle, simplifying the pipeline structure. And facilitate the manufacturing and installation of the system. In the delivery needle assembly of the present disclosure, preferably, the plurality of holes are disposed proximate the third end of the second channel.
在本公开的输送针组件中，较佳地，所述孔包括多个围绕所述第二通道成圈排列在所述外壁上的孔组，所述孔组之间沿所述外壁的纵向方向间隔预定距离，和/或所述孔在所述外壁中相对于所述第二通道的纵向方向垂直或使得所述孔的径向外侧相较所述孔的径向内侧更靠近所述第三端地倾斜布置。孔的这些布置方式有助于高效地对容器内壁进行残留样品收集，避免样品残留死角，尽可能减少样品在制备过程的中缺损。In the delivery needle assembly of the present disclosure, preferably, the holes include a plurality of hole groups arranged in a circle on the outer wall around the second channel, and between the hole groups along the longitudinal direction of the outer wall spaced at a predetermined distance, and/or the holes are perpendicular to the longitudinal direction of the second channel in the outer wall or such that the radially outer side of the hole is closer to the third than the radially inner side of the hole. End-to-end tilted arrangement. These arrangements of holes help to efficiently collect residual samples from the inner wall of the container, avoid dead corners of sample residues, and minimize sample defects during the preparation process.
较佳地，孔的孔径在0.2-0.3mm之间。该孔径大小有利于形成微滴。Preferably, the hole diameter is between 0.2-0.3mm. This pore size facilitates droplet formation.
在本公开的输送针组件中，较佳地，在所述第二通道的所述第三端，所述外壁通过焊接部固定到所述内壁，焊接部使所述第二通道的第三端封闭。焊接部能够实现两个通道的可靠连接和密封。In the delivery needle assembly of the present disclosure, preferably, at the third end of the second channel, the outer wall is fixed to the inner wall through a welding portion, and the welding portion makes the third end of the second channel closed. The welded part enables reliable connection and sealing of the two channels.
附图说明Description of the drawings
为了能更完全理解本公开，可参考结合附图来考虑示例性实施例的下述描述，附图中：For a more complete understanding of the present disclosure, reference may be made to the following description of exemplary embodiments taken in conjunction with the accompanying drawings, in which:
图1示出了根据本公开较佳实施例的用于对样品进行蒸发的***的示意框图。Figure 1 shows a schematic block diagram of a system for evaporating a sample according to a preferred embodiment of the present disclosure.
图2示出了根据本公开较佳实施例的配合安装到容器的输送针装置的示意图。Figure 2 shows a schematic diagram of a delivery needle device fitted to a container according to a preferred embodiment of the present disclosure.
图3A示出了根据本公开较佳实施例的输送针的立体图。Figure 3A shows a perspective view of a delivery needle according to a preferred embodiment of the present disclosure.
图3B示出了图3A所示输送针的两个端部的放大立体图。 Figure 3B shows an enlarged perspective view of both ends of the delivery needle shown in Figure 3A.
图4示出了根据本公开较佳实施例的输送针的一部分的纵向截面的剖视图。Figure 4 shows a cross-sectional view of a longitudinal section of a portion of a delivery needle in accordance with a preferred embodiment of the present disclosure.
图5示出了以图4中A-A向剖取的剖视图。FIG. 5 shows a cross-sectional view taken along the A-A direction in FIG. 4 .
图6示出了以图4中B-B向剖取的剖视图。FIG. 6 shows a cross-sectional view taken along the B-B direction in FIG. 4 .
图7A示出了通过如图3A所示的输送针向容器输送待蒸发样品的示意图。Figure 7A shows a schematic diagram of delivering a sample to be evaporated to a container through a delivery needle as shown in Figure 3A.
图7B示出了在样品蒸发的同时通过如图3A所示的输送针向容器提供气体的示意图。Figure 7B shows a schematic diagram of providing gas to a container through a delivery needle as shown in Figure 3A while the sample is evaporating.
图7C示出了通过如图3A所示的输送针对容器的内壁进行残留样品收集的示意图。Figure 7C shows a schematic diagram of residual sample collection on the inner wall of the container by the delivery needle as shown in Figure 3A.
图8A示出了根据一较佳实施例的输送针的端部的放大立体图。Figure 8A shows an enlarged perspective view of the end of a delivery needle according to a preferred embodiment.
图8B示出了根据另一较佳实施例的输送针的端部的放大立体图。Figure 8B shows an enlarged perspective view of the end of a delivery needle according to another preferred embodiment.
图9示出了根据一较佳实施例的对样品进行蒸发的方法的步骤流程图。Figure 9 shows a step flow chart of a method for evaporating a sample according to a preferred embodiment.
附图标记列表List of reference signs
用于对样品进行蒸发的***System for evaporating samples
10溶剂提供装置10Solvent supply device
20气体提供装置20 gas supply device
30样品提供装置30 sample supply device
31控制阀31 control valve
40切换机构40 switching mechanism
50负压施加装置50 negative pressure application device
60输送针装置60 delivery needle device
61移动保持件61 mobile retainer
62 O形圈62 O-ring
63衬垫63 pads
64固定保持件64 fixed retainer
65、66保持件通道65, 66 retainer channel
67 O形圈67 O-ring
70输送针70 delivery needle
71第一通道 71 first channel
72第二通道72 second channel
75第一管件75 first pipe fittings
76第二管件76 second pipe fitting
77孔77 holes
78保持架78 cage
80封盖80 blocks
90容器90 containers
91容器口91 container mouth
110溶剂提供管路110 solvent supply pipeline
120气体提供管路120 gas supply pipeline
150旁通管路150 bypass line
具体实施方式Detailed ways
下面结合具体实施例和附图对本公开作进一步说明，在以下的描述中阐述了更多的细节以便于充分理解本公开，但是本公开显然能够以多种不同于此描述的其它方式来实施，本领域技术人员可以在不违背本公开内涵的情况下根据实际应用情况作类似推广、演绎，因此不应以此具体实施例的内容限制本公开的保护范围。The present disclosure will be further described below in conjunction with specific embodiments and drawings. More details are set forth in the following description in order to fully understand the present disclosure. However, the present disclosure can obviously be implemented in a variety of other ways that are different from this description. Those skilled in the art can make similar generalizations and deductions based on actual application conditions without violating the connotation of the present disclosure. Therefore, the protection scope of the present disclosure should not be limited by the content of the specific embodiments.
图1示出了根据本公开较佳实施例的用于对样品进行蒸发的***的示意框图。需要被蒸发处理的样品借助于容器放置在该***中，***用于加热容器，使容器内的液态样品的温度升高，由此使样品中可蒸发的成份逸出，从而达到样品浓缩或干燥的目的。同时，该***还能够向蒸发的样品施加压力气体，以加速浓缩或干燥的过程。Figure 1 shows a schematic block diagram of a system for evaporating a sample according to a preferred embodiment of the present disclosure. The sample that needs to be evaporated is placed in the system with the help of a container. The system is used to heat the container to increase the temperature of the liquid sample in the container, thereby allowing the evaporable components in the sample to escape, thereby concentrating or drying the sample. the goal of. At the same time, the system can also apply pressure gas to the evaporated sample to accelerate the concentration or drying process.
本领域技术人员理解，在很多情况下，必须将待分析的目的化学品(即，分析物)从物质中提取出来，以使得可以用对应检测技术对其进行例如定性或定量的分析检测。比如，可以通过固液萃取的方法进行此类提取，从固体或半固体物质中溶解出分析物。固体或半固体物质可以是含有分析物的任何材料或基质，例如药品、土壤、或食品等。本发明中的“分析物”从固体或半固体物质中分离出的后续可用于分析技术检测(例如定性或定量)的化学品，例如药品中的活性成分、土壤中的农药、或食品中的脂质。本发明中的“样品”指的是含有分析物的液体溶剂，可以送入蒸发装置进行浓缩。以来自固液萃取的样 品为例，其应当包含从固体或半固体物质中溶出的分析物。Those skilled in the art understand that in many cases, the target chemical to be analyzed (ie, the analyte) must be extracted from the substance so that it can be analyzed and detected, for example, qualitatively or quantitatively, using corresponding detection techniques. For example, this type of extraction can be performed by solid-liquid extraction, which dissolves analytes from solid or semi-solid materials. A solid or semi-solid substance can be any material or matrix containing an analyte, such as pharmaceuticals, soil, or food. The "analyte" in the present invention is a chemical that is separated from a solid or semi-solid substance and can subsequently be used for analytical technology detection (such as qualitative or quantitative), such as active ingredients in pharmaceuticals, pesticides in soil, or chemicals in food. Lipids. The "sample" in the present invention refers to the liquid solvent containing the analyte, which can be sent to the evaporation device for concentration. Samples from solid-liquid extraction For example, products should contain analytes leached from solid or semi-solid materials.
如图1所示，用于对样品进行蒸发的***主要包括样品提供装置30、气体提供装置20、溶剂提供装置10、切换机构40以及输送针装置60。各提供装置10、20、30流体联通地连接到输送针装置60，液态样品、气体和溶剂通过输送针装置60送入到置于***中的容器90内。As shown in FIG. 1 , the system for evaporating samples mainly includes a sample providing device 30 , a gas providing device 20 , a solvent providing device 10 , a switching mechanism 40 and a delivery needle device 60 . Each providing device 10, 20, 30 is fluidly connected to a delivery needle device 60 through which liquid samples, gases and solvents are delivered into a container 90 placed in the system.
图1示例性地示出了四个容器90，每一个容器配置一个输送针装置60。FIG. 1 shows by way of example four containers 90 , each container being assigned a delivery needle device 60 .
***中的样品提供装置30构造成用于向置于***内的容器90提供待蒸发的样品。应当理解，***中的样品提供装置30可以包括任何类型的能够向容器提供样品装置。通常，样品提供装置30包括容纳待蒸发的样品的贮存部和输送机构。样品提供装置30中提供的样品可以是在装置30中直接制备完成并由装置30提供到容器90，也可以是以其他独立样品制备装置制备完成后装入样品提供装置再提供到容器90。The sample providing device 30 in the system is configured for providing a sample to be evaporated to a container 90 placed within the system. It will be appreciated that the sample providing device 30 in the system may comprise any type of device capable of providing a sample to a container. Typically, the sample providing device 30 includes a storage portion for receiving the sample to be evaporated and a transport mechanism. The sample provided in the sample providing device 30 may be directly prepared in the device 30 and provided to the container 90 by the device 30 , or may be prepared by another independent sample preparation device and then loaded into the sample providing device and then provided to the container 90 .
在一较佳实施方式中，样品提供装置30可以构造成加速溶剂萃取的装置，它主要包括一个或多个加热萃取单元。在样品提供装置30中，含有分析物的固体或半固体物质被置于加热萃取单元中，来自溶剂提供装置10的溶剂被送入加热萃取单元，随着单元的温度和压力的升高，分析物析出到溶剂中，从而萃取获得液态样品，以供后续蒸发使用。In a preferred embodiment, the sample providing device 30 may be configured as a device for accelerating solvent extraction, which mainly includes one or more heated extraction units. In the sample providing device 30, the solid or semi-solid material containing the analyte is placed in the heated extraction unit, and the solvent from the solvent providing device 10 is sent into the heated extraction unit. As the temperature and pressure of the unit increase, the analysis The material is precipitated into the solvent, thereby extracting a liquid sample for subsequent evaporation.
图1示出的样品提供装置30包括四个加热萃取单元，每一个加热萃取单元通过控制阀31连接到一个输送针装置60。应当理解，加热萃取单元的数量可以更多或更少，加热萃取单元的数量可设置成与输送针装置60的数量对应。The sample providing device 30 shown in FIG. 1 includes four heated extraction units, each heated extraction unit being connected to a delivery needle device 60 through a control valve 31 . It should be understood that the number of heated extraction units may be more or less, and the number of heated extraction units may be configured to correspond to the number of delivery needle devices 60 .
***中的气体提供装置20构造成用于向样品提供装置30提供气体，以加速样品提供装置30的萃取。气体提供装置20也能够通过输送针装置60不经过样品提供装置30直接向容器90提供气体。沿着气体输送路径，样品提供装置30布置在气体提供装置20和容器90之间，可以通过气体提供装置20经过样品提供装置30向容器90输送气体。The gas providing device 20 in the system is configured to provide gas to the sample providing device 30 to accelerate extraction by the sample providing device 30 . The gas supply device 20 can also directly supply gas to the container 90 through the delivery needle device 60 without passing through the sample supply device 30 . Along the gas delivery path, the sample providing device 30 is arranged between the gas providing device 20 and the container 90 , and the gas can be delivered to the container 90 by the gas providing device 20 through the sample providing device 30 .
气体提供装置20所提供的气体通常为惰性气体，例如氮气。在样品蒸发过程中，气体提供装置20可以向容器90吹入氮气，即实现氮吹功能，从而使样品挥发速度加快，减少蒸发时间。另一方面，在容器内壁残留样品收集的过程中，气体提供装置20提供气体能够用于使液体的加速且分散，形成喷射流体或雾状液体施加到容器90的内壁，以实现内壁的残留样品收集。气体提供装置20较佳地被构造成能够提供350到500Psi压力范围的气体，这一压力范 围的气体将适用于***的加速蒸发及容器残留样品收集过程。The gas provided by the gas supply device 20 is usually an inert gas, such as nitrogen. During the evaporation process of the sample, the gas supply device 20 can blow nitrogen into the container 90 , thereby realizing the nitrogen blowing function, thereby speeding up the evaporation of the sample and reducing the evaporation time. On the other hand, during the process of collecting residual samples on the inner wall of the container, the gas supply device 20 provides gas that can be used to accelerate and disperse the liquid to form a spray fluid or mist liquid and apply it to the inner wall of the container 90 to achieve residual samples on the inner wall. collect. The gas supply device 20 is preferably configured to provide gas in a pressure range of 350 to 500 Psi. The surrounding gas will be suitable for the accelerated evaporation of the system and the collection of residual samples from the container.
此外，***中包括的溶剂提供装置10构造成用于向置于***内的容器90提供溶剂，并且也用于向样品提供装置30提供溶剂以对各类分析物进行溶剂萃取操作。In addition, the solvent supply device 10 included in the system is configured to provide solvent to a container 90 disposed within the system, and also to provide solvent to the sample supply device 30 for performing solvent extraction operations on various types of analytes.
***中的切换机构40构造成用于实现不同模式下的流路选择，使溶剂和气体根据***执行的操作步骤的需要被输送到输送针的相应通道(下文中将详述)。The switching mechanism 40 in the system is configured to realize flow path selection in different modes, so that solvent and gas are transported to corresponding channels of the delivery needle according to the needs of the operating steps performed by the system (to be described in detail below).
如图1所示，溶剂提供装置10包括溶剂提供管路110，而气体提供装置20包括气体提供管路120，溶剂提供管路110和气体提供管路120分别流体连通到切换机构40。较佳地，切换机构40包括电子旋转阀(ERV阀)。较佳地，电子旋转阀包括至少一个入口端、至少两个出口端以及选择地连通该入口端及一个出口端的旋转切换阀。入口端可操作地连通气体提供装置20和溶剂提供装置10，而一个出口端与样品提供装置30相连并进而连接到输送针装置中的输送针的第一通道，而另一个出口端与输送针装置中的输送针的第二通道相连。通过控制旋转切换阀，可以选择性地将入口端与选中的出口端连通，从而实现不同模式下的流路选择。As shown in FIG. 1 , the solvent supply device 10 includes a solvent supply pipeline 110 , and the gas supply device 20 includes a gas supply pipeline 120 . The solvent supply pipeline 110 and the gas supply pipeline 120 are respectively fluidly connected to the switching mechanism 40 . Preferably, the switching mechanism 40 includes an electronic rotary valve (ERV valve). Preferably, the electronic rotary valve includes at least one inlet end, at least two outlet ends, and a rotary switching valve that selectively communicates with the inlet end and one outlet end. The inlet end is operably connected to the gas supply device 20 and the solvent supply device 10, while one outlet end is connected to the sample supply device 30 and thereby to the first channel of the delivery needle in the delivery needle device, and the other outlet end is connected to the delivery needle. The second channel of the delivery needle in the device is connected. By controlling the rotary switching valve, the inlet end can be selectively connected to the selected outlet end, thereby realizing flow path selection in different modes.
对于图1所示的四个样品提供装置30和四个输送针装置60的***，电子旋转阀可具有一个入口端和八个出口端，其中四个出口端分别连接一个样品提供装置30以可选的向对应的输送针70的第一通道输送气体或溶剂，而另四个出口端分别连接到输送针装置中以可选的向对应的输送针70的第二通道输送气体或溶剂。For the system of four sample providing devices 30 and four delivery needle devices 60 shown in FIG. 1 , the electronic rotary valve may have one inlet end and eight outlet ends, wherein the four outlet ends are respectively connected to one sample providing device 30 to allow Gas or solvent is selectively delivered to the first channel of the corresponding delivery needle 70 , while the other four outlet ends are respectively connected to the delivery needle device to optionally deliver gas or solvent to the second channel of the corresponding delivery needle 70 .
在本***中设置切换机构40简化了溶剂和气体的输送管路布置。应当理解，在其他替代实施例中，切换机构40可以包括单向阀和控制阀，溶剂提供装置10和气体提供装置20分别通过各自单独连接的管路上的单向阀和控制阀来实现向样品提供装置30和容器90输送溶剂和气体的控制。Providing the switching mechanism 40 in this system simplifies the arrangement of the solvent and gas delivery pipelines. It should be understood that in other alternative embodiments, the switching mechanism 40 may include a one-way valve and a control valve, and the solvent supply device 10 and the gas supply device 20 realize supply to the sample through the one-way valves and control valves on their respective individually connected pipelines. Control of the delivery of solvents and gases to the device 30 and container 90 is provided.
样品提供装置30设置在切换机构40的下游，而输送针装置60及容器90进一步设置在样品提供装置30的下游，这样，来自溶剂提供装置10的溶剂和来自气体提供装置20的气体通过切换机构40可被输送到样品提供装置30。当在操作中需要将气体送入容器90时，来自气体提供装置20的气体可以通过切换机构40流经样品提供装置30和输送针装置60进入容器90。The sample providing device 30 is disposed downstream of the switching mechanism 40, and the delivery needle device 60 and the container 90 are further disposed downstream of the sample providing device 30. In this way, the solvent from the solvent providing device 10 and the gas from the gas providing device 20 pass through the switching mechanism. 40 may be transported to sample providing device 30. When gas needs to be fed into the container 90 during operation, the gas from the gas supply device 20 can flow through the sample supply device 30 and the delivery needle device 60 into the container 90 through the switching mechanism 40 .
本领域技术人员可以理解，在特定步骤中，根据不同需求，来自气体提 供装置20的气体也可以不经过切换机构40直接进入样品提供装置30，并流经输送针装置60进入容器90.Those skilled in the art can understand that in specific steps, according to different needs, from gas extraction The gas from the supply device 20 can also directly enter the sample supply device 30 without passing through the switching mechanism 40, and flow through the delivery needle device 60 into the container 90.
另一方面，如图1所示，切换机构40与输送针装置60之间连接着一旁通管路150，该旁通管路150不经过样品提供装置30。在切换机构40的控制切换下，来自溶剂提供装置10的溶剂将绕开样品提供装置30经由旁通管路150直接送达输送针装置60，进入容器90。On the other hand, as shown in FIG. 1 , a bypass line 150 is connected between the switching mechanism 40 and the delivery needle device 60 , and the bypass line 150 does not pass through the sample supply device 30 . Under the control switching of the switching mechanism 40 , the solvent from the solvent supply device 10 will bypass the sample supply device 30 and pass through the bypass line 150 directly to the delivery needle device 60 and enter the container 90 .
***中输送针装置60构造成配合多种规格的容器90使用，该装置60能够保持并移动输送针，用于向容器输送气体、液体或气液混合物。The delivery needle device 60 in the system is configured to be used with containers 90 of various specifications. The device 60 can hold and move the delivery needle for delivering gas, liquid or gas-liquid mixture to the container.
容器90可以构造为具有各种不同的容量，例如60ml、100ml、250ml等。容器90可以构造为具有各种不同的形状，例如如图2所示的仅顶部具有容器口91的平底瓶形状，如图7B所示的中间大两头小且两头且上下具有开口的形状，其中下端的开口适于配接小瓶(例如，2ml容量小瓶)，以便接纳小容量的蒸发后收集到的样品。可选的，容器与小瓶之间可以通过适配器配接。Container 90 may be configured with various capacities, such as 60ml, 100ml, 250ml, etc. The container 90 can be configured to have various shapes, such as a flat-bottom bottle shape with only a container opening 91 on the top as shown in Figure 2, a shape with a large center and two small ends and openings at both ends and upper and lower ends as shown in Figure 7B, where The opening at the lower end is adapted to fit a vial (for example, a 2 ml capacity vial) to receive a small volume of sample collected after evaporation. Optionally, the container and vial can be connected via an adapter.
图2示出了较佳实施例的输送针装置60以及与输送针装置60配合使用的容器90。输送针装置60主要包括输送针70、移动保持件61、使输送针70上下移动的移动机构、固定保持件64以及封盖80。如图2所示，移动保持件61固Figure 2 illustrates a preferred embodiment delivery needle device 60 and a container 90 for use with the delivery needle device 60. The delivery needle device 60 mainly includes a delivery needle 70, a moving holder 61, a moving mechanism for moving the delivery needle 70 up and down, a fixed holder 64, and a cover 80. As shown in Figure 2, the mobile retainer 61 is fixed
定保持输送针70的上部，而固定保持件64滑动地保持输送针70的中下部，这两个保持件61和64都起到了保持输送针70的作用。其中移动保持件61是一个可动部件，固定保持件64是一个固定不动的部件，通过两者的相对移动，输送针70实现上下移动。The upper part of the delivery needle 70 is fixedly held, and the fixed holding member 64 slides to hold the middle and lower part of the delivery needle 70 . Both holding parts 61 and 64 play a role in holding the delivery needle 70 . The movable holding part 61 is a movable part, and the fixed holding part 64 is a fixed part. Through the relative movement of the two, the delivery needle 70 moves up and down.
输送针装置60的移动保持件61和驱动器被作为输送针70的移动机构，其中移动保持件61构造成保持输送针70。驱动器则附连到移动保持件61使移动保持件61相对下方的固定保持件64上下运动，从而使得输送针70穿过固定保持件64和封盖80能够相对容器作上下移动。在较佳实施例中，驱动器较佳地为电机。The movement holder 61 and the drive of the delivery needle device 60 serve as a movement mechanism for the delivery needle 70 , the movement holder 61 being configured to hold the delivery needle 70 . The driver is attached to the moving holder 61 to move the movable holder 61 up and down relative to the fixed holder 64 below, so that the delivery needle 70 passes through the fixed holder 64 and the closure 80 can move up and down relative to the container. In a preferred embodiment, the driver is preferably a motor.
应当理解，在其他替代实施方式中，输送针装置60也以可以其他方式来移动输送针，例如驱动器直接附连到输送针使之移动。It should be understood that in other alternative embodiments, the delivery needle device 60 may move the delivery needle in other ways, such as with a driver attached directly to the delivery needle to move it.
移动机构的设置可以使得***能够适配于不同规格的容器使用，也可以使得通过允许输送针位于不同高度来实现进样、容器内壁残留样品收集及通过气吹加速蒸发等不同功能，从而使得***整体适配性强，且结构紧凑，节省实 验室内有限的操作空间。The setting of the moving mechanism can make the system adaptable to containers of different specifications, and can also allow the delivery needle to be located at different heights to achieve different functions such as sample injection, collection of residual samples on the inner wall of the container, and accelerated evaporation through air blowing, thus making the system The overall adaptability is strong, and the structure is compact, saving real-time Limited operating space in the laboratory.
较佳地，固定保持件64与输送针70之间设有一个或多个诸如O形圈67的密封件以实现滑动密封。Preferably, one or more seals such as O-rings 67 are provided between the fixed retainer 64 and the delivery needle 70 to achieve a sliding seal.
在较佳实施例中，相对于同一规格的容器，移动机构可以设定成输送针70可移动到以下位置的部分或全部：不执行任何操作的原始位置、输送针70向容器提供样品的位置、输送针70向容器施加气液混合物的位置以及输送针70在容器加热时输送气体的位置(以下称第一位置)。通常，第一位置低于输送针70开始向容器施加气体和溶剂的位置。这样提供溶剂和气体时输送针的位置相对输送气体进行气吹的第一位置更高，因此，通过输送针向容器内施加流体进行残留样品收集时具有较高位置，这有助于相对全面地覆盖容器内壁，使得对容器内壁残留样品的收集更为完整输送针进行气吹的第一位置相对较低，这样输送针能够将气体送到较为靠近容器内待蒸发液态样品的位置，有利于加速样品的蒸发。此外，输送针70向容器施加气液混合物的位置较佳地设定成高于输送针70向容器提供样品的位置。这样的位置设定有助于使输送针70施加气液混合物能够更全面覆盖当输送针提供样品时飞溅到容器内壁而残留的样品。In a preferred embodiment, relative to containers of the same specification, the moving mechanism can be set so that the delivery needle 70 can move to part or all of the following positions: an original position where no operation is performed, and a position where the delivery needle 70 provides samples to the container. , the position where the delivery needle 70 applies the gas-liquid mixture to the container, and the position where the delivery needle 70 delivers gas when the container is heated (hereinafter referred to as the first position). Typically, the first position is lower than where the delivery needle 70 begins to apply gas and solvent to the container. In this way, the position of the delivery needle when supplying solvent and gas is higher than the first position of delivering gas for air blowing. Therefore, the delivery needle has a higher position when applying fluid into the container for residual sample collection, which helps to relatively comprehensively Covering the inner wall of the container makes the collection of residual samples on the inner wall of the container more complete. The first position of the delivery needle for air blowing is relatively low, so that the delivery needle can send the gas to a position closer to the liquid sample to be evaporated in the container, which is beneficial to acceleration. Evaporation of sample. In addition, the position where the delivery needle 70 applies the gas-liquid mixture to the container is preferably set higher than the position where the delivery needle 70 provides the sample to the container. Such a position setting helps the delivery needle 70 to apply the gas-liquid mixture to more comprehensively cover the remaining sample that splashes onto the inner wall of the container when the delivery needle provides the sample.
当容器90置于***内时，输送针装置60可通过封盖80的至少一部分附连到容器90的容器口91，如图2所示，封盖80的下方凸出部***地附连到容器口91中，输送针70的一端延伸通过容器90的容器口91并且通过封盖80中的通孔***容器90内部，并且封盖80与输送针70之间设有多个诸如O形圈62的密封件以实现密封，输送针70相对于封盖80是可移动的。封盖8相对于容器口91之间应形成密封配合，以防流体外逸。为了实现密封配合，在在较佳实施例中，封盖80与容器口91之间可以附加诸如由弹性材料制成的衬垫63，封盖80将衬垫63压靠在容器口91上，这将有助于实现封盖80与容器口91之间的密封配合。When the container 90 is placed within the system, the delivery needle device 60 may be attached to the container mouth 91 of the container 90 through at least a portion of the closure 80 , as shown in FIG. 2 , the lower projection of the closure 80 being insertably attached to In the container mouth 91, one end of the delivery needle 70 extends through the container mouth 91 of the container 90 and is inserted into the interior of the container 90 through the through hole in the cover 80, and a plurality of O-rings such as O-rings are provided between the cover 80 and the delivery needle 70. 62 to achieve sealing, the delivery needle 70 is movable relative to the cover 80. The lid 8 should form a sealing fit relative to the container mouth 91 to prevent fluid from escaping. In order to achieve a sealing fit, in a preferred embodiment, a liner 63 made of elastic material can be added between the cover 80 and the container mouth 91, and the cover 80 presses the liner 63 against the container mouth 91. This will help achieve a sealing fit between the closure 80 and the container mouth 91 .
为了在***中执行样品进样、容器内壁残留样品收集以及蒸发气吹，输送针70至少包括第一通道71和第二通道72，第二通道72位于第一通道71的外侧，两个通道71和72是相互隔开的，从而能够独立地输送流体。In order to perform sample injection, collection of residual samples on the inner wall of the container, and evaporation gas blowing in the system, the delivery needle 70 at least includes a first channel 71 and a second channel 72 , the second channel 72 is located outside the first channel 71 , and the two channels 71 and 72 are spaced apart from each other to enable independent fluid delivery.
图4具体示出了双层结构的输送针70。输送针70包括第一管件75和第二管件76，第二管件76围绕着第一管件75，两个管件75和76较佳地基本同心设置。这样，在该较佳实施例，第一通道71由内层第一管件75的中空空 间构成，第二通道72由第二管件76与第一管件75之间的管状空间构成。这样，第二通道72围绕着第一通道71，两个通道71、72之间通过至少一个壁隔开。FIG. 4 specifically shows the delivery needle 70 with a double-layer structure. The delivery needle 70 includes a first tube member 75 and a second tube member 76. The second tube member 76 surrounds the first tube member 75. The two tube members 75 and 76 are preferably substantially concentrically arranged. In this way, in this preferred embodiment, the first channel 71 is formed by the hollow space of the inner first pipe member 75. The second channel 72 is composed of a tubular space between the second pipe member 76 and the first pipe member 75 . In this way, the second channel 72 surrounds the first channel 71, and the two channels 71, 72 are separated by at least one wall.
沿着输送针70的纵向方向，第一通道71具有可伸入容器90的第一端和连通到样品提供装置30的第二端，第二通道72具有可伸入容器90的第三端和可切换地连通到气体提供装置20的溶剂提供装置10的第四端。第一通道71具有设置在第一端的开口，换言之，第一管件75的第一端是敞开的。Along the longitudinal direction of the delivery needle 70, the first channel 71 has a first end that can extend into the container 90 and a second end that is connected to the sample providing device 30, and the second channel 72 has a third end that can extend into the container 90 and The fourth end of the solvent supply device 10 is switchably connected to the gas supply device 20 . The first channel 71 has an opening disposed at a first end, in other words, the first end of the first tube 75 is open.
在较佳实施例中，第一管件75的该敞开的端部的端面可以设置成倾斜面，如图8A所示。在另一替代较佳实施例中，第一管件75的端部的可沿着管件的纵向方向开设槽口，如图8B所示。In a preferred embodiment, the end surface of the open end of the first tube 75 may be configured as an inclined surface, as shown in FIG. 8A . In another alternative preferred embodiment, the end of the first tube 75 may be notched along the longitudinal direction of the tube, as shown in Figure 8B.
特别地，输送针70的第二通道72的第三端是封闭的，换言之，第二管件76具有位于第三端的封闭端部。In particular, the third end of the second channel 72 of the delivery needle 70 is closed, in other words, the second tube 76 has a closed end at the third end.
在较佳实施例中，如图4所示，第一管件75和第二管件76之间通过焊接组装连接，形成一体式的输送针。较佳地，第二管件76的与第二通道72的第三端对应的端部通过焊接部固定到第一管件75的外表面上，焊接部使得第二通道72的该第三端封闭。In a preferred embodiment, as shown in Figure 4, the first pipe member 75 and the second pipe member 76 are assembled and connected through welding to form an integrated delivery needle. Preferably, the end of the second pipe member 76 corresponding to the third end of the second channel 72 is fixed to the outer surface of the first pipe member 75 through a welding portion, and the welding portion causes the third end of the second channel 72 to be closed.
在输送针70的另一端处，如图3B所示，输送针70还可包括一个保持架78。该保持架78分别固定地附连到第一管件75和第二管件76，以使保持两个管件之间的相对位置。较佳地，保持架78包括固定附连到第二管件76的端部的环和从环内部延伸出固定地附连到第一管件75的外表面的多个连接筋。保持架78与第一管件75和第二管件76之间较佳地也通过焊接固定。At the other end of the delivery needle 70, as shown in Figure 3B, the delivery needle 70 may also include a retainer 78. The cage 78 is fixedly attached to the first tube 75 and the second tube 76 respectively, so as to maintain the relative position between the two tubes. Preferably, the retainer 78 includes a ring fixedly attached to the end of the second tube 76 and a plurality of connecting ribs extending from the interior of the ring fixedly attached to the outer surface of the first tube 75 . The cage 78 and the first pipe member 75 and the second pipe member 76 are preferably also fixed by welding.
在形成第二通道72的第二管件76的外壁中，在靠近第二通道72的第三端的位置处设有多个孔77，这些孔77使得第二通道72与外部连通，以允许溶剂或气体通过这些孔77进出。第二通道72的外壁中的这些孔77的用途是允许流体喷出以对容器90内壁进行残留样品收集，避免样品在制备过程中缺损。通常，流体为压缩气体与溶剂结合形成的气液混合物，一部分气液混合物会在气体压力的作用下直接喷射到容器的内壁，随后液体沿内壁流下，带走内壁上可能存在的残留物；另一部分溶剂会在高压气体的作用下雾化，在容器内部空间形成微液滴，微液滴会附着到内壁沿内壁流下，雾化部分的溶剂能够补充覆盖喷射施加未能覆盖的那部分内壁表面，使得容器内壁的残留样品收集更充分。压缩气体的压力通常可以被控制在350-500Psi的压力的范围中，这一压 力范围对于充分清除容器内壁上的残留物是有利的。In the outer wall of the second tube 76 forming the second channel 72, a plurality of holes 77 are provided near the third end of the second channel 72. These holes 77 allow the second channel 72 to communicate with the outside to allow solvent or Gas enters and exits through these holes 77 . The purpose of these holes 77 in the outer wall of the second channel 72 is to allow the fluid to be ejected to collect residual samples on the inner wall of the container 90 to avoid sample damage during the preparation process. Usually, the fluid is a gas-liquid mixture formed by a combination of compressed gas and solvent. Part of the gas-liquid mixture will be directly sprayed to the inner wall of the container under the action of gas pressure, and then the liquid will flow down along the inner wall, taking away any residue that may be present on the inner wall; Part of the solvent will be atomized under the action of high-pressure gas, forming micro droplets in the internal space of the container. The micro droplets will adhere to the inner wall and flow down the inner wall. The atomized part of the solvent can supplement the surface of the inner wall that is not covered by the spray application. , allowing the residual samples on the inner wall of the container to be collected more fully. The pressure of compressed gas can usually be controlled in the range of 350-500Psi. This pressure The force range is favorable for adequate removal of residues from the inner walls of the container.
多个孔77围绕第二通道72成圈排列成，在外壁形成多圈孔组。多圈孔组之间沿第二通道72的外壁的纵向方向以预定距离隔开。在图4所示的实施例中，优选的，多个孔77排列形成两圈孔组。每圈孔组具有12个孔，每圈孔组中的多个孔77彼此在所述外壁的周向方向中等间距地隔开。The plurality of holes 77 are arranged in a circle around the second channel 72 to form a multi-circle hole group on the outer wall. The plurality of hole groups are spaced apart at a predetermined distance along the longitudinal direction of the outer wall of the second channel 72 . In the embodiment shown in FIG. 4 , preferably, the plurality of holes 77 are arranged to form two circles of hole groups. Each hole group has 12 holes, and the plurality of holes 77 in each hole group are evenly spaced from each other in the circumferential direction of the outer wall.
在图4所示的实施例中，孔77在管件壁中的延伸方向相对于输送针70的纵向轴线成90度。但应当理解，也可设想将这些孔77在管件的壁的延伸方向相对于输送针70的纵向轴线(即输送针的纵向方向)向着输送针7的图2所示的下端倾斜布置，使得孔77的径向外侧相较孔77的径向内侧更靠近位于下方的第三端，这样喷射出的流体会有一个朝向容器90底部的分量，当流体施加到容器90内壁上后，向下分量能够加速流体沿容器90内壁向下流动，提高残留样品收集效果。In the embodiment shown in FIG. 4 , the hole 77 extends in the wall of the tube at 90 degrees relative to the longitudinal axis of the delivery needle 70 . However, it should be understood that it is also conceivable to arrange these holes 77 obliquely in the extension direction of the wall of the tube relative to the longitudinal axis of the delivery needle 70 (ie the longitudinal direction of the delivery needle) towards the lower end of the delivery needle 7 shown in Figure 2, so that the holes The radially outer side of 77 is closer to the lower third end than the radial inner side of hole 77, so that the ejected fluid will have a component toward the bottom of container 90. When the fluid is applied to the inner wall of container 90, there will be a downward component. It can accelerate the downward flow of fluid along the inner wall of the container 90 and improve the residual sample collection effect.
从图5和图6中可以看到，两圈孔组中孔77的分布位置并不一定沿输送针的纵向方向对齐的，如图6所示，靠近第三端的一圈孔组中的一个孔77和远离第三端的一圈孔组中的与之最接近的一个孔77的两者的径向中心线之间在周向偏置一角度α，例如α为15度，这样，当通过孔77喷射液体对容器内壁进行残留样品收集时，可以使内壁残留样品收集覆盖范围更全更完整，避免出现残留有样品的死角。It can be seen from Figures 5 and 6 that the distribution positions of the holes 77 in the two hole groups are not necessarily aligned along the longitudinal direction of the delivery needle. As shown in Figure 6, one of the hole groups in the circle near the third end The radial center lines of the hole 77 and the closest hole 77 in a circle of holes away from the third end are circumferentially offset by an angle α, for example, α is 15 degrees. In this way, when passing When the hole 77 sprays liquid to collect residual samples on the inner wall of the container, the collection coverage of the residual samples on the inner wall can be more complete and complete, and avoid dead corners with residual samples.
应当理解，输送针70的孔77数量可以更多或更少，较佳地，每一圈孔组的在8到16个孔之间。较佳地，输送针70的第二通道72上的孔77的孔径d1可以设定在0.2-0.3mm之间，较佳地为0.25mm。这一范围孔径的孔77有利于在喷射的同形时形成雾化的微液滴，从而实现同时以射流和雾化微液滴的两种方式使溶剂施加到容器内壁，从而使得内壁覆盖得更全面。输送针的第三端的开口的孔径d2可以设定在0.8-1.2mm之间，较佳地为1mm。第一管件75的外壁面和第二管件76的内壁面之间的间距可以在0.3-0.5mm之间。It should be understood that the number of holes 77 of the delivery needle 70 can be more or less, preferably, each circle of hole groups has between 8 and 16 holes. Preferably, the aperture d1 of the hole 77 on the second channel 72 of the delivery needle 70 can be set between 0.2-0.3 mm, preferably 0.25 mm. The holes 77 with apertures in this range are conducive to the formation of atomized micro-droplets when spraying in the same shape, thereby enabling the solvent to be applied to the inner wall of the container in two ways: jet flow and atomized micro-droplets at the same time, thereby making the inner wall more covered. comprehensive. The aperture d2 of the opening of the third end of the delivery needle can be set between 0.8-1.2 mm, preferably 1 mm. The distance between the outer wall surface of the first pipe member 75 and the inner wall surface of the second pipe member 76 may be between 0.3-0.5 mm.
在根据本公开的较佳实施例中，输送针装置60的输送针70包括第一通道71和位于第一通道71外侧的第二通道72。如图2所示，移动保持件61中设有至少两个保持件通道65、66。其中一条保持件通道65的一端与输送针70的第一通道71连通，保持件通道65的另一端连通到样品提供装置30并且经由样品提供装置30和切换机构40连通到气体提供装置20和溶剂提供装置10。另一条保持件通道66的一端与输送针70的第二通道72连通，该通道66的另 一端则通过管路连接到切换机构40的一个出口端，从而分别可操作地连通气体提供装置20和溶剂提供装置10。由此，通过输送针装置60，第一通道71可与样品提供装置30流体相连，并且第一通道71可选地与气体提供装置20流体相连，并且，第二通道72可选地与溶剂提供装置10或气体提供装置20流体相连。In a preferred embodiment according to the present disclosure, the delivery needle 70 of the delivery needle device 60 includes a first channel 71 and a second channel 72 located outside the first channel 71 . As shown in Figure 2, at least two holder channels 65, 66 are provided in the mobile holder 61. One end of one of the holder channels 65 is connected to the first channel 71 of the delivery needle 70 , and the other end of the holder channel 65 is connected to the sample providing device 30 and is connected to the gas providing device 20 and the solvent via the sample providing device 30 and the switching mechanism 40 Apparatus 10 is provided. One end of the other holder channel 66 is connected to the second channel 72 of the delivery needle 70, and the other end of the channel 66 is connected to the second channel 72 of the delivery needle 70. One end is connected to an outlet end of the switching mechanism 40 through a pipeline, thereby operatively communicating with the gas supply device 20 and the solvent supply device 10 respectively. Thus, the first channel 71 can be in fluid communication with the sample supply device 30 via the delivery needle device 60, and the first channel 71 can optionally be in fluid communication with the gas supply device 20, and the second channel 72 can optionally be in fluid communication with the solvent supply device. The device 10 or the gas supply device 20 is fluidly connected.
为了对样品和溶液通过第一通道71和第二通道72的流动进行控制，在一个优先实施例中，切换机构40被构造成至少具有第一切换位置、第二切换位置和第三切换位置。在第一切换位置，第一通道71经由样品提供装置30与气体提供装置20流体相连；在第二切换位置，第二通道72绕开样品提供装置30通过旁通管路150直接与气体提供装置20流体相连；在第三切换位置，第二通道72通过旁通管路150绕开样品提供装置30直接与所述溶剂提供装置流体相连。In order to control the flow of samples and solutions through the first channel 71 and the second channel 72, in a preferred embodiment, the switching mechanism 40 is configured to have at least a first switching position, a second switching position and a third switching position. In the first switching position, the first channel 71 is fluidly connected to the gas providing device 20 via the sample providing device 30; in the second switching position, the second channel 72 bypasses the sample providing device 30 and is directly connected to the gas providing device through the bypass line 150. 20 is fluidly connected; in the third switching position, the second channel 72 bypasses the sample providing device 30 and is directly fluidly connected to the solvent providing device through the bypass line 150 .
此外，所述***还可包括用于第二通道72的切断装置，该切断装置构造成当第一通道71与样品提供装置30流体相连时封闭第二通道72，以避免容器内的气体流第二通道72反流流出***。例如，切断装置可以是安装在与第二通道72连通的保持件通道66中的切断阀。In addition, the system may further include a shut-off device for the second channel 72, the shut-off device being configured to close the second channel 72 when the first channel 71 is in fluid connection with the sample providing device 30 to avoid gas flow within the container. Two-channel 72 reflux outflow system. For example, the shut-off device may be a shut-off valve installed in the holder channel 66 that communicates with the second channel 72 .
具体而言，如图1所示，样品提供装置30布置在输送针装置60的上游，两者之间设置有输送管路，因此，样品提供装置30中的获得样品能够经该输送管路输送针装置中的保持件通道65流入第一通道71。可选地，气体提供装置20中的气体通过气体提供管路120、切换机构40、样品提供装置30以及保持件通道65流入第一通道71。本领域技术人员可以理解，在特定步骤中，根据不同需求，来自气体提供装置20的气体也可以不经过切换机构40直接进入样品提供装置30，并流经保持件通道65，流入第一通道71。另一方面，来自气体提供装置20的气体或者来自溶剂提供装置10的溶剂通过切换机构40流过旁通管路150、通过输送针装置60中的保持件通道66送到输送针的第二通道72中，以执行相应的操作步骤。Specifically, as shown in FIG. 1 , the sample providing device 30 is arranged upstream of the delivery needle device 60 with a delivery pipeline between the two. Therefore, the sample obtained in the sample providing device 30 can be delivered through the delivery pipeline. The holder channel 65 in the needle device flows into the first channel 71 . Optionally, the gas in the gas supply device 20 flows into the first channel 71 through the gas supply pipe 120 , the switching mechanism 40 , the sample supply device 30 and the holder channel 65 . Those skilled in the art can understand that in a specific step, according to different requirements, the gas from the gas supply device 20 can also directly enter the sample supply device 30 without passing through the switching mechanism 40 , and flow through the holder channel 65 and into the first channel 71 . On the other hand, the gas from the gas supply device 20 or the solvent from the solvent supply device 10 flows through the bypass line 150 through the switching mechanism 40 and is sent to the second channel of the delivery needle through the holder channel 66 in the delivery needle device 60 72 to perform the corresponding steps.
进一步如图1所示，用于样品蒸发的***还包括负压施加装置50。该负压施加装置50连通到容器90，以便对容器90提供负压，例如，抽真空。较佳地，可以在附连到容器90的封盖80上设置连接负压施加装置50的负压端口，负压施加装置50可以通过该连接端口连接。As further shown in FIG. 1 , the system for sample evaporation also includes a negative pressure application device 50 . The negative pressure applying device 50 is connected to the container 90 to provide negative pressure to the container 90, for example, to evacuate. Preferably, a negative pressure port connected to the negative pressure applying device 50 may be provided on the cover 80 attached to the container 90, and the negative pressure applying device 50 may be connected through the connection port.
此外，较佳地，在蒸发过程中，从容器90逸出的气体也可以通过负压端 口排出。***还可包括废气回收装置，封盖80上的负压端口可以连接到废气回收装置，从而使废气被回收，避免逸出气体对环境造成污染以及对人体造成伤害。本领域技术人员可以理解，容器90的封盖80上也可以设置独立的废气端口，用于逸出气体的排出。In addition, preferably, during the evaporation process, the gas escaping from the container 90 can also pass through the negative pressure end Mouth discharge. The system may also include a waste gas recovery device, and the negative pressure port on the cover 80 may be connected to the waste gas recovery device, so that the waste gas can be recovered to avoid pollution of the environment and harm to the human body caused by the escaped gas. Those skilled in the art can understand that an independent exhaust gas port can also be provided on the cover 80 of the container 90 for the discharge of escaped gas.
接着，参照图7A、图7B和图7C以及图9对根据较佳实施例的对容器中样品执行的具体步骤进行说明。图9示出了根据本公开较佳实施例的对样品进行蒸发的方法的步骤流程图Next, the specific steps performed on the sample in the container according to the preferred embodiment will be described with reference to FIGS. 7A, 7B, 7C and 9. Figure 9 shows a step flow chart of a method for evaporating a sample according to a preferred embodiment of the present disclosure.
具体而言，图9所示的较佳的方法流程包括：将输送针移动到向容器提供样品的位置的步骤S100、通过输送针向容器提供待蒸发样品的步骤S102、将输送针移动到向容器内壁施加溶剂和气体的位置的步骤S104、向容器内壁施加溶剂和气体的步骤S106、使输送针移动到施加气体的第一位置的步骤S108、使容器内的样品蒸发的步骤S110以及通过输送针向容器提供来自气体提供装置的气体的步骤S112。如图9中步骤S112后所示，样品在S114处处于已制备完成状态。上述使容器内的样品蒸发的步骤S110是指***执行至少一个手段实现蒸发的步骤，例如通过加热进行蒸发。应当理解图9所示的流程仅是示例性的，流程中并非每一个步骤都必须的，也不一定必须按图9所示步骤的前后次序执行。通过输送针向容器提供待蒸发样品的步骤S102和使容器内的样品蒸发的步骤S110可以同时开始执行。但在替代实施例，步骤S110也可以步骤S102开始一段时间但未完全结束，或者步骤S102结束之后开始执行。例如，输送针可以不移动而直接执行通过输送针向容器提供待蒸发样品的步骤S102。又例如，通过输送针向容器提供来自气体提供装置的气体的步骤S112被可以省略，而仅执行使容器内的样品蒸发的步骤S110来实现样品蒸发浓缩。Specifically, the preferred method flow shown in Figure 9 includes: step S100 of moving the delivery needle to a position for providing a sample to the container, step S102 of providing a sample to be evaporated to the container through the delivery needle, and moving the delivery needle to a position where the sample is provided to the container. Step S104 of applying solvent and gas to the inner wall of the container, step S106 of applying solvent and gas to the inner wall of the container, step S108 of moving the delivery needle to the first position of applying gas, step S110 of evaporating the sample in the container, and by conveying Step S112 of supplying gas from the gas supply device to the container. As shown after step S112 in Figure 9, the sample is in a prepared state at S114. The above-mentioned step S110 of evaporating the sample in the container refers to a step in which the system performs at least one means to achieve evaporation, such as evaporation through heating. It should be understood that the process shown in Figure 9 is only exemplary, and not every step in the process is necessary, nor does it necessarily have to be performed in the order of the steps shown in Figure 9 . The step S102 of providing the sample to be evaporated to the container through the delivery needle and the step S110 of evaporating the sample in the container may be started simultaneously. However, in alternative embodiments, step S110 may also be executed for a period of time starting from step S102 but not completely completed, or may be executed after step S102 is completed. For example, the delivery needle may not move but directly perform the step S102 of providing the sample to be evaporated to the container through the delivery needle. For another example, step S112 of providing gas from the gas supply device to the container through a delivery needle can be omitted, and only step S110 of evaporating the sample in the container is performed to achieve sample evaporation concentration.
在执行通过输送针70向容器901提供待蒸发样品的步骤S102中，如图7A所示，***通过输送针70位于内侧的第一通道71从样品提供装置30向容器901提供待蒸发的样品。进入容器901的样品可以是通过溶剂萃取分析物即时获得的。在输送样品时，从气体提供装置20通入样品提供装置30的一部分气体也会随着样品一同被送入容器901。随着流体从第一通道71送入容器，容器901中多余的气体会通过封盖80的废气端口逸出，较佳地被收集到废气回收装置，容器901内部的压力被释放。In step S102 of providing the sample to be evaporated to the container 901 through the delivery needle 70 , as shown in FIG. 7A , the system provides the sample to be evaporated from the sample providing device 30 to the container 901 through the first channel 71 located inside the delivery needle 70 . Samples entering container 901 may be obtained instantaneously by solvent extraction of the analytes. When transporting the sample, part of the gas flowing from the gas supply device 20 into the sample supply device 30 will also be sent into the container 901 together with the sample. As the fluid is fed into the container from the first channel 71, excess gas in the container 901 will escape through the exhaust port of the cover 80, and is preferably collected into an exhaust gas recovery device, and the pressure inside the container 901 will be released.
在执行通过输送针70向容器提供待蒸发样品的步骤S102之前，根据使用容器的需要，可选地执行将输送针70移动到向容器提供样品的位置的步骤 S100。在该步骤S100中，输送针装置60的移动机构将输送针70从原位移动到执行向容器提供样品的一个特定位置。输送针70的原始位置通常是输送针70的下端接近于封盖80的一个位置。相比输送针70的原始位置，如图7A所示的输送针执行向容器提供样品的位置更低，因此输送针70竖直向下移动。输送针提供样品的位置较佳地被设置在容器的颈缩肩部下方的一个合适位置处。图7A和图7B示出了两种不同规格的容器901和902，对于执行输送针向容器提供待蒸发样品的步骤，可以理解，输送针70从原始位置向下移动的距离是不同的，具体移动距离可根据容器901和902的不同高度来设定。Before performing the step S102 of providing the sample to be evaporated to the container through the delivery needle 70, according to the needs of using the container, the step of moving the delivery needle 70 to a position for providing the sample to the container is optionally performed. S100. In this step S100, the moving mechanism of the delivery needle device 60 moves the delivery needle 70 from the original position to a specific position where sample supply to the container is performed. The original position of the delivery needle 70 is usually a position where the lower end of the delivery needle 70 is close to the cover 80 . Compared to the original position of the delivery needle 70 , the delivery needle as shown in FIG. 7A performs supplying the sample to the container at a lower position, so the delivery needle 70 moves vertically downward. The point at which the delivery needle delivers the sample is preferably located at a suitable location below the necked shoulder of the container. Figure 7A and Figure 7B show two different specifications of containers 901 and 902. Regarding the step of performing the step of providing the sample to be evaporated by the delivery needle to the container, it can be understood that the distance the delivery needle 70 moves downward from the original position is different. Specifically, The moving distance can be set according to the different heights of containers 901 and 902.
图7C示意性地示出了向容器内壁施加溶剂和气体的步骤S106。施加流体到内壁是为了尽可能多地收集容器901内壁上残留的样品，避免由于样品在内壁上的残留导致最终样品分析误差。这些样品残余可能是在样品送入容器901时飞溅到内壁上，或是在样品液位降低过程中附着在容器901内壁的。Figure 7C schematically shows step S106 of applying solvent and gas to the inner wall of the container. The purpose of applying fluid to the inner wall is to collect as much sample remaining on the inner wall of the container 901 as possible to avoid final sample analysis errors due to sample residue on the inner wall. These sample residues may be splashed onto the inner wall of the container 901 when the sample is fed into the container 901, or may be attached to the inner wall of the container 901 during the lowering of the sample liquid level.
根据本公开的较佳实施例，向容器901内壁施加流体的操作步骤是通过输送针70的第二通道72进行的。在施加溶剂和气体的步骤S106中，首先从溶剂提供装置10经过旁通管路150向输送针70的第二通道72提供溶剂。此时，溶剂并没有完全从第二通道72的外壁中的孔离开第二通道72，而是至少有部分滞留在第二通道72中或者与第二通道72相连的管路中。接着，气体提供装置20经过旁通管路150向第二通道72提供压缩气体，压缩气体将作用在滞留在管路中的溶剂，使气体与溶剂结合形成气液混合物并通出第二通道72的孔77，施加到容器901的内壁上。According to a preferred embodiment of the present disclosure, the step of applying fluid to the inner wall of the container 901 is performed through the second channel 72 of the delivery needle 70 . In step S106 of applying the solvent and gas, the solvent is first supplied from the solvent supply device 10 to the second channel 72 of the delivery needle 70 through the bypass line 150 . At this time, the solvent does not completely leave the second channel 72 through the holes in the outer wall of the second channel 72 , but is at least partially retained in the second channel 72 or in the pipeline connected to the second channel 72 . Next, the gas supply device 20 provides compressed gas to the second channel 72 through the bypass pipeline 150. The compressed gas will act on the solvent remaining in the pipeline, causing the gas and the solvent to combine to form a gas-liquid mixture and flow out of the second channel 72. holes 77, applied to the inner wall of the container 901.
在上述步骤S106中，溶剂从第二通道72的孔77喷射而出，由于采用高压气体，一部分溶剂在气体压力的作用下直接喷射到容器901的内壁上，液体沿内壁流下，带走内壁上可能存在的残留物；另一部分溶剂会在气体的压力下雾化，在容器901内部形成微液滴，微液滴附着到内壁并沿内壁流下。因此理解，采用这一步骤S106，仅需向第二通道72提供少量的溶剂，就能够有效地对容器内壁进行残留样品收集。在该步骤S106中，压缩气体的压力可以被控制在350-500Psi的压力的范围中，这一压力范围对于充分清除容器内壁上的残留物是有利的。In the above step S106, the solvent is ejected from the hole 77 of the second channel 72. Due to the use of high-pressure gas, a part of the solvent is directly ejected onto the inner wall of the container 901 under the action of gas pressure, and the liquid flows down along the inner wall and is taken away from the inner wall. There may be residues; another part of the solvent will be atomized under the pressure of the gas, forming micro droplets inside the container 901, and the micro droplets will adhere to the inner wall and flow down along the inner wall. Therefore, it is understood that by using this step S106, only a small amount of solvent is required to be provided to the second channel 72 to effectively collect residual samples from the inner wall of the container. In this step S106, the pressure of the compressed gas can be controlled in a pressure range of 350-500 Psi. This pressure range is beneficial for fully removing residues on the inner wall of the container.
应当理解，在向容器内壁施加溶剂和气体的操作步骤S106中，溶剂通过切换机构40与输送针装置60之间的旁通管路150朝着输送针70的第二通道72送出，这部分溶剂不会经过样品提供装置30。在该步骤中被送到容器901 内的溶剂无需通过样品提供装置30提供，这样的设计缩短了溶剂被施加到容器内壁前所经过的流动距离，从而减少了流路中阻力可能产生的影响，使得在向容器内壁施加溶剂和气体时，溶剂所受的力被更精确地控制，达到更好的清洗内壁的效果。此外，流动距离的缩短也使得在该步骤中被送到容器901内的溶剂的量可以被相对精确计量。It should be understood that in the operation step S106 of applying solvent and gas to the inner wall of the container, the solvent is sent out toward the second channel 72 of the delivery needle 70 through the bypass line 150 between the switching mechanism 40 and the delivery needle device 60. This part of the solvent It does not pass through the sample providing device 30. Sent to container 901 in this step The solvent in the container does not need to be provided through the sample providing device 30. This design shortens the flow distance that the solvent travels before being applied to the inner wall of the container, thereby reducing the possible impact of resistance in the flow path, so that when the solvent and gas are applied to the inner wall of the container At this time, the force on the solvent is more accurately controlled to achieve better cleaning effect on the inner wall. In addition, the shortening of the flow distance also allows the amount of solvent sent into the container 901 in this step to be measured relatively accurately.
在替代实施例中，向容器内壁施加溶剂和气体的步骤S106可以重复执行多次，即，先由溶剂提供装置10向第二通道72提供少量溶剂，随即由气体提供装置20通过旁通管路150输送压缩气体，向容器内壁面实施一次喷射，紧接着或间隔一段时间，再次执行溶剂提供装置10向第二通道72提供少量溶剂和由气体提供装置20输送压缩气体的操作，实施二次喷射。喷射的数量可以根据容器的规格和样品的种类确定。In an alternative embodiment, the step S106 of applying solvent and gas to the inner wall of the container can be repeated multiple times, that is, a small amount of solvent is first provided by the solvent supply device 10 to the second channel 72, and then the gas supply device 20 passes through the bypass line. 150 delivers compressed gas, and performs one injection to the inner wall of the container. Immediately or after a period of time, the solvent supply device 10 provides a small amount of solvent to the second channel 72 and the gas supply device 20 delivers the compressed gas again to perform a second injection. . The number of injections can be determined according to the size of the container and the type of sample.
优选地，在执行向容器901内壁施加溶剂和气体的操作步骤S106之前，可选地将输送针移动到向容器内壁施加溶剂和气体的位置的步骤S104。在该步骤S104中，输送针装置60中的移动机构将输送针70移动到向容器内壁施加溶剂和气体的位置，例如如图7C所示的位置，输送针70向容器内壁施加溶剂和气体的位置较佳地设置在容器的颈缩肩部下方或附近。Preferably, before performing the operation step S106 of applying solvent and gas to the inner wall of the container 901, there is optionally a step S104 of moving the delivery needle to a position for applying solvent and gas to the inner wall of the container. In this step S104, the moving mechanism in the delivery needle device 60 moves the delivery needle 70 to a position where solvent and gas are applied to the inner wall of the container, such as the position shown in FIG. 7C, where the delivery needle 70 applies solvent and gas to the inner wall of the container. The location is preferably below or near the necked shoulder of the container.
较佳地，对于同一规格的容器，图7C所示的输送针70向内壁施加溶剂和气体的位置比如图7A所示的输送针提供样品的位置稍高。同样地，输送针70向内壁施加溶剂和气体的位置可以根据选用的容器的规格不同而利用程序进行设定。Preferably, for containers of the same specification, the position where the delivery needle 70 shown in FIG. 7C applies solvent and gas to the inner wall is slightly higher than the position where the delivery needle 70 shown in FIG. 7A provides the sample. Likewise, the position where the delivery needle 70 applies solvent and gas to the inner wall can be set using a program according to the specifications of the selected container.
在其他替代实施例中，对于同一规格的容器，输送针向容器内壁施加溶剂和气体的位置和通过输送针向容器提供待蒸发样品的位置可以是同一位置，在这种情况下，步骤S104可以省略。In other alternative embodiments, for containers of the same specification, the position where the delivery needle applies solvent and gas to the inner wall of the container and the position where the sample to be evaporated is provided to the container through the delivery needle may be the same position. In this case, step S104 may be Omit.
较佳地，如图9所示，向容器901提供待蒸发样品的步骤S102开始的同时，可以执行使容器内的样品蒸发的步骤S110，这样可以减少样品制备的总时长。在这种情况下，向容器内壁施加溶剂和气体的步骤S106同样也在使容器内的样品蒸发的步骤S110进行的同时执行。Preferably, as shown in FIG. 9 , when the step S102 of providing the sample to be evaporated to the container 901 is started, the step S110 of evaporating the sample in the container can be performed, which can reduce the total time of sample preparation. In this case, step S106 of applying solvent and gas to the inner wall of the container is also performed simultaneously with step S110 of evaporating the sample in the container.
在一个替代实施例中，可以向容器901提供待蒸发样品的步骤S102并且在向容器内壁施加溶剂和气体的步骤S106完成之后，执行使容器内的样品蒸发的步骤S110。In an alternative embodiment, the step S102 of providing the sample to be evaporated to the container 901 and the step S110 of evaporating the sample within the container may be performed after the step S106 of applying solvent and gas to the inner wall of the container is completed.
在其他替代实施例中，也可以省略前述两个步骤S102和S106，步骤S110 可以在例如操作人员手动将装载着待蒸发的样品的容器放置到***内后直接进行。In other alternative embodiments, the aforementioned two steps S102 and S106 and step S110 may also be omitted. This can be done, for example, directly after the operator manually places the container containing the sample to be evaporated into the system.
为了加速蒸发，可选地执行通过输送针向容器提供来自气体提供装置的气体的步骤S112。在该步骤S112中，通过输送针70的第一通道71向容器901提供来自气体提供装置20的气体。气体较佳地为氮气，氮气以一定压力提供，该压力通常在350-500Psi的范围内。In order to accelerate evaporation, step S112 of supplying gas from the gas supply device to the container through the delivery needle is optionally performed. In this step S112, the gas from the gas supply device 20 is supplied to the container 901 through the first channel 71 of the delivery needle 70. The gas is preferably nitrogen, which is provided at a certain pressure, usually in the range of 350-500 Psi.
在较佳实施例中，通过输送针向容器提供来自气体提供装置的气体的步骤S112可以在向容器901提供待蒸发样品的步骤S102和向容器内壁施加溶剂和气体的步骤S106完成之后开始，此时，使容器内的样品蒸发的步骤S110正在进行。或者，在替代实施方式中，步骤S112可以与使容器内的样品蒸发的步骤S110的步骤同时开始。步骤S112较佳地持续执行到样品蒸发完成，但也可以设定一段执行时间，在样品蒸发完成前结束步骤S112。In a preferred embodiment, the step S112 of providing the gas from the gas supply device to the container through the delivery needle can be started after the step S102 of providing the sample to be evaporated to the container 901 and the step S106 of applying the solvent and gas to the inner wall of the container. When , the step S110 of evaporating the sample in the container is in progress. Alternatively, in an alternative embodiment, step S112 may be initiated simultaneously with the step of evaporating the sample within the container S110. Step S112 is preferably continued until the sample evaporation is completed, but a period of execution time may also be set to end step S112 before the sample evaporation is completed.
为了在通过输送针向容器提供来自气体提供装置的气体的步骤S112中使气体集中作用到容器的液态样品上，较佳地，可以在执行通过输送针向容器提供来自气体提供装置的气体的步骤S112之前执行使输送针移动到施加气体的第一位置的步骤S108。在步骤S108中，移动机构可以使输送针70移动到针对特定规格的容器设定的通过第一通道施加气体的第一位置，该第一位置相比输送针施加溶剂和气体的位置和向容器提供待蒸发样品的位置更低。通常，该步骤在如图7B所示的两端开口、在下端附连小瓶的容器使用时执行，输送针70在第一位置时，输送针70的下端接近容器下方开口。输送针70的第一通道71能够施加氮吹到容器的样品内中，从而实现样品的无氧浓缩，从而可以保证样品的纯净度，并加速蒸发。In order to concentrate the gas on the liquid sample in the container in the step S112 of supplying the gas from the gas supply device to the container through the delivery needle, it is preferable to perform the step of supplying the gas from the gas supply device to the container through the delivery needle. Step S108 of moving the delivery needle to a first position for applying gas is performed before S112. In step S108, the moving mechanism may move the delivery needle 70 to a first position for applying gas through the first channel set for a container of a specific specification. The first position is compared to a position where the delivery needle applies solvent and gas to the container. The position where the sample to be evaporated is provided is lower. Typically, this step is performed when a container with openings at both ends and a vial attached at the lower end as shown in FIG. 7B is used. When the delivery needle 70 is in the first position, the lower end of the delivery needle 70 is close to the lower opening of the container. The first channel 71 of the delivery needle 70 can apply nitrogen to blow into the sample in the container, thereby achieving oxygen-free concentration of the sample, thus ensuring the purity of the sample and accelerating evaporation.
最后，当容器内的样品浓缩达到设定要求后，***将停止加热容器，等***内部充分冷却、温度降低到安全值后，便可从***中取出制备好的样品，从而获得目标样品。Finally, when the concentration of the sample in the container reaches the set requirement, the system will stop heating the container. After the inside of the system is fully cooled and the temperature drops to a safe value, the prepared sample can be taken out of the system to obtain the target sample.
对于常规的进样蒸发样品的操作，***可以通过设定相应的时间、温度等相应参数，对多样品且自动执行输送针向容器提供待蒸发样品的步骤S102、向容器内壁施加溶剂和气体的步骤S106以及使容器内的样品蒸发S110的步骤。For the conventional operation of injecting and evaporating samples, the system can automatically perform the step S102 of providing the sample to be evaporated by the delivery needle to the container for multiple samples, and applying solvent and gas to the inner wall of the container by setting corresponding parameters such as time and temperature. Step S106 and the step of evaporating the sample in the container S110.
但应当理解，***的控制装置或控制方法也可以被设置成能够可选地执行其输送针向容器提供待蒸发样品的步骤S102、向容器内壁施加溶剂和气体的步骤S106以及加热容器使容器内的样品蒸发的步骤S110中的任一项步骤，以满 足某些情况下样品制备的特殊需求。However, it should be understood that the control device or control method of the system can also be configured to optionally perform the step S102 of providing the sample to be evaporated to the container by its delivery needle, the step S106 of applying solvent and gas to the inner wall of the container, and heating the container to make the inside of the container Any one of the steps in step S110 of sample evaporation is required to satisfy Meet the special needs of sample preparation in some cases.
在其他替代实施例中，输送针70也可以在第一通道71和第二通道72之间还可能包括一个或多个第三通道。例如，该第三通道被设置成与溶剂提供装置10、气体提供装置20以及样品提供装置30中的一个或多个流体连通，以执行附加操作。In other alternative embodiments, the delivery needle 70 may also include one or more third channels between the first channel 71 and the second channel 72 . For example, the third channel is provided in fluid communication with one or more of the solvent providing device 10, the gas providing device 20, and the sample providing device 30 to perform additional operations.
又或者，第三通道可以与废气回收装置或负压施加装置连通，负压的施加或废气的回收可以通过第三通道实施。Alternatively, the third channel may be connected to an exhaust gas recovery device or a negative pressure application device, and the application of negative pressure or the recovery of exhaust gas may be implemented through the third channel.
本公开虽然以较佳实施例公开如上，但其并不是用来限定本公开，任何本领域技术人员在不脱离本公开的精神和范围内，都可以做出可能的变动和修改。因此，凡是未脱离本公开技术方案的内容，依据本公开的技术实质对以上实施例所作的任何修改、等同变化及修饰，均落入本公开权利要求所界定的保护范围之内。 Although the present disclosure is disclosed above in terms of preferred embodiments, this is not intended to limit the present disclosure. Any person skilled in the art can make possible changes and modifications without departing from the spirit and scope of the present disclosure. Therefore, any modifications, equivalent changes and modifications made to the above embodiments based on the technical essence of the present disclosure that do not deviate from the technical solution of the present disclosure shall fall within the protection scope defined by the claims of the present disclosure.

Claims (21)

  1. 一种对容器中样品进行蒸发的方法，A method of evaporating a sample in a container,
    所述方法包括：The methods include:
    -通过输送针向所述容器提供待蒸发样品，所述输送针包括第一通道和第二通道，所述第二通道位于所述第一通道的外侧，且所述输送针形成第二通道的外壁具有多个孔，所述样品通过所述第一通道进入所述容器；- Provide the sample to be evaporated to the container through a delivery needle, the delivery needle comprising a first channel and a second channel, the second channel being located outside the first channel, and the delivery needle forming a second channel The outer wall has a plurality of holes, and the sample enters the container through the first channel;
    -向所述第二通道提供溶剂和气体，以使位于所述第二通道中的溶剂通过所述孔施加至所述容器的内壁；以及- supplying solvent and gas to the second channel so that the solvent located in the second channel is applied to the inner wall of the container through the holes; and
    -加热所述容器，使所述容器内的样品蒸发，在进行所述加热的过程中，可选地通过所述第一通道向所述容器提供气体。- heating the container to evaporate the sample within the container, optionally supplying gas to the container through the first channel during said heating.
  2. 如权利要求1所述的方法，其特征在于，提供溶剂和气体的步骤还依次包括：The method of claim 1, wherein the steps of providing solvent and gas further include:
    -向所述第二通道提供溶剂；- providing solvent to said second channel;
    -在所述溶剂离开所述第二通道的孔之前向所述第二通道提供气体，使所述气体与所述溶剂结合形成气液混合物并通出所述孔。- Providing gas to the second channel before the solvent leaves the hole of the second channel so that the gas combines with the solvent to form a gas-liquid mixture and passes out of the hole.
  3. 如权利要求2所述的方法，其特征在于，提供溶剂和气体步骤还包括：The method of claim 2, wherein the step of providing solvent and gas further includes:
    -将经压缩的气体施加到所述溶剂，使所述气液混合物通出所述孔后形成微滴，所述微滴的至少一部分被施加到所述容器的内壁上。- Applying compressed gas to the solvent, allowing the gas-liquid mixture to pass through the hole to form droplets, at least a portion of the droplets being applied to the inner wall of the container.
  4. 如权利要求1所述的方法，其特征在于，提供溶剂和气体步骤后还包括：The method according to claim 1, characterized in that after the step of providing solvent and gas, it further includes:
    -将所述输送针向下移动到第一位置，所述第一位置低于所述输送针在执行所述提供溶剂和气体步骤时所处位置；- moving the delivery needle downward to a first position lower than the position of the delivery needle when performing the step of providing solvent and gas;
    并且所述输送针向下移动步骤后还包括：And after the step of moving the transport needle downward, it also includes:
    -通过所述第一通道向所述容器提供气体。- supplying gas to the container through the first channel.
  5. 如权利要求4所述的方法，其特征在于，所述加热容器使所述容器内的样品蒸发的步骤与所述通过第一通道向容器提供待蒸发样品的步骤同时开始执行。 The method of claim 4, wherein the step of heating the container to evaporate the sample in the container is started simultaneously with the step of providing the sample to be evaporated to the container through the first channel.
  6. 如权利要求1所述的方法，其特征在于，加热所述容器使所述容器内的样品蒸发的步骤进一步包括：The method of claim 1, wherein the step of heating the container to evaporate the sample in the container further includes:
    -当通过所述第一通道向所述容器提供气体时，封闭所述第二通道。- closing the second channel when gas is supplied to the container through the first channel.
  7. 一种对样品进行蒸发的***，包括：A system for evaporating samples consisting of:
    样品提供装置，所述样品提供装置向容器提供所述样品；a sample providing device that provides the sample to the container;
    气体提供装置，所述气体提供装置向所述容器提供气体；a gas supply device that provides gas to the container;
    溶剂提供装置，所述溶剂提供装置向所述容器提供溶剂；a solvent supply device that provides solvent to the container;
    加热装置，所述加热装置构造成加热所述容器中的所述样品；以及a heating device configured to heat the sample in the container; and
    输送针装置，所述输送针装置包括输送针，所述输送针包括第一通道和第二通道，所述第二通道位于所述第一通道的外侧，形成所述第二通道的外壁具有多个孔，Delivery needle device, the delivery needle device includes a delivery needle, the delivery needle includes a first channel and a second channel, the second channel is located outside the first channel, and the outer wall forming the second channel has multiple a hole,
    其中所述输送针装置构造成使所述第一通道与所述样品提供装置流体相连，且所述第一通道可选地与所述气体提供装置流体相连，并且所述输送针装置构造成使所述第二通道可选地与所述溶剂提供装置或所述气体提供装置流体相连。wherein the delivery needle device is configured to fluidly connect the first channel to the sample providing device, and the first channel is optionally in fluid communication to the gas providing device, and the delivery needle device is configured to fluidly connect the first channel to the sample providing device. The second channel is optionally in fluid communication with the solvent provider or the gas provider.
  8. 如权利要求7所述的***，其特征在于，所述输送针装置包括使所述输送针相对所述容器上下移动的移动机构。The system of claim 7, wherein the delivery needle device includes a moving mechanism for moving the delivery needle up and down relative to the container.
  9. 如权利要求8所述的***，其特征在于，The system of claim 8, wherein:
    所述移动机构构造成在所述第一通道与所述气体提供装置流体相连的情况下使所述输送针移动到第一位置，所述第一位置低于当所述第二通道可选地与所述溶剂提供装置或所述气体提供装置流体相连时所述输送针所处位置。The movement mechanism is configured to move the delivery needle to a first position with the first channel in fluid communication with the gas provider, the first position being lower than when the second channel optionally The position of the delivery needle when in fluid connection with the solvent provider or the gas provider.
  10. 如权利要求7所述的***，其特征在于，所述输送针装置包括封盖，所述第一通道和所述第二通道密封地穿过所述封盖，所述封盖构造成密封地配合到容器的容器口，且所述输送针相对所述封盖可移动。7. The system of claim 7, wherein the delivery needle device includes a cover, the first channel and the second channel sealingly extending through the cover, the cover being configured to sealingly pass through the cover. Fitted to the container mouth of the container, and the delivery needle is movable relative to the closure.
  11. 如权利要求10所述的***，其特征在于，所述***进一步包括负压施 加装置和/或废气回收装置，The system of claim 10, further comprising a negative pressure application addition device and/or exhaust gas recovery device,
    所述封盖设有连接到所述负压施加装置和/或所述废气回收装置的端口。The cover is provided with a port connected to the negative pressure applying device and/or the exhaust gas recovery device.
  12. 如权利要求7所述的***，其特征在于，The system of claim 7, wherein:
    所述***包括切换机构，The system includes a switching mechanism,
    所述第一通道经由所述样品提供装置和所述切换机构流体连接到所述气体提供装置，the first channel is fluidly connected to the gas provider via the sample provider and the switching mechanism,
    所述第二通道经由所述切换机构与所述气体提供装置和所述溶剂提供装置分别流体相连，the second channel is fluidly connected to the gas supply device and the solvent supply device respectively via the switching mechanism,
    所述切换机构具有第一切换位置、第二切换位置和第三切换位置，The switching mechanism has a first switching position, a second switching position and a third switching position,
    在所述第一切换位置，所述第一通道经由所述样品提供装置与所述气体提供装置流体相连；In the first switching position, the first channel is fluidly connected to the gas providing device via the sample providing device;
    在所述第二切换位置，所述第二通道绕开所述样品提供装置直接与所述气体提供装置流体相连；In the second switching position, the second channel bypasses the sample providing device and is directly fluidly connected to the gas providing device;
    在所述第三切换位置，所述第二通道绕开所述样品提供装置直接与所述溶剂提供装置流体相连。In the third switching position, the second channel bypasses the sample providing device and is directly fluidly connected to the solvent providing device.
  13. 如权利要求12所述的***，其特征在于，所述***包括用于所述第二通道的切断装置，所述切断装置构造成当所述第一通道与所述样品提供装置流体相连时封闭所述第二通道。12. The system of claim 12, including a shutoff device for the second channel, the shutoff device being configured to close when the first channel is in fluid communication with the sample providing device. The second channel.
  14. 如权利要求7所述的***，其特征在于，所述气体提供装置设置成以350-500Psi的压力向所述容器提供气体。The system of claim 7, wherein the gas supply device is configured to provide gas to the container at a pressure of 350-500 psi.
  15. 如权利要求7所述的***，其特征在于，所述输送针还包括第三通道，所述第三通道介于所述第一通道和所述第二通道之间The system of claim 7, wherein the delivery needle further includes a third channel, the third channel being between the first channel and the second channel.
    所述第三通道可选地与所述溶剂提供装置或所述气体提供装置流体相连。The third channel is optionally in fluid communication with the solvent provider or the gas provider.
  16. 一种用于蒸发***的输送针组件，包括：A delivery needle assembly for an evaporation system, including:
    第一通道，所述第一通道具有第一端和第二端；a first channel having a first end and a second end;
    第二通道，所述第二通道具有第三端和第四端，所述第二通道位于所述第 一通道的外侧；以及a second channel, the second channel having a third end and a fourth end, the second channel being located at the the outside of a channel; and
    封盖，所述第一通道和所述第二通道密封地穿过所述封盖，所述封盖构造成密封地配合到容器的容器口；a closure through which the first channel and the second channel sealingly extend, the closure being configured to sealingly fit to a container mouth of the container;
    其特征在于，It is characterized by,
    所述第一通道具有设置在所述第一端的开口；The first channel has an opening disposed at the first end;
    所述第二通道的所述第三端封闭，形成所述第二通道的外壁具有多个孔，所述多个孔使得通出所述第二通道的气液混合物被雾化为微液滴并被施加到所述容器的内壁。The third end of the second channel is closed, and the outer wall forming the second channel has a plurality of holes. The plurality of holes allow the gas-liquid mixture passing through the second channel to be atomized into micro droplets. and is applied to the inner wall of the container.
  17. 如权利要求16所述的输送针组件，其特征在于，所述第二通道围绕所述第一通道，所述第二通道与所述第一通道通过至少一内壁隔开，The delivery needle assembly of claim 16, wherein the second channel surrounds the first channel, and the second channel is separated from the first channel by at least one inner wall,
    其中所述外壁和所述内壁固定为一体。The outer wall and the inner wall are fixed as one body.
  18. 如权利要求16所述的输送针组件，其特征在于，The delivery needle assembly of claim 16, wherein:
    所述多个孔靠近所述第二通道的所述第三端设置。The plurality of holes are disposed proximate the third end of the second channel.
  19. 如权利要求16所述的输送针组件，其特征在于，The delivery needle assembly of claim 16, wherein:
    所述孔包括多个围绕所述第二通道成圈排列在所述外壁上的孔组，所述孔组之间沿所述外壁的纵向方向间隔预定距离，和/或所述孔在所述外壁中相对于所述第二通道的纵向方向垂直或使得所述孔的径向外侧相较所述孔的径向内侧更靠近所述第三端地倾斜布置。The holes include a plurality of hole groups arranged in a circle on the outer wall around the second channel, the hole groups are spaced apart at a predetermined distance along the longitudinal direction of the outer wall, and/or the holes are on the outer wall. The outer wall is arranged perpendicularly with respect to the longitudinal direction of the second channel or so that the radially outer side of the hole is closer to the third end than the radially inner side of the hole.
  20. 如权利要求16所述的输送针组件，其特征在于，The delivery needle assembly of claim 16, wherein:
    所述孔的孔径在0.2-0.3mm之间。The diameter of the hole is between 0.2-0.3mm.
  21. 如权利要求17所述的输送针组件，其特征在于，在所述第二通道的所述第三端，所述外壁通过焊接部固定到所述内壁，所述焊接部使所述第二通道的第三端封闭。 The delivery needle assembly of claim 17, wherein at the third end of the second channel, the outer wall is secured to the inner wall by a weld, the weld causing the second channel to The third end is closed.
PCT/CN2023/100369 2022-06-16 2023-06-15 System and method for evaporating sample, and delivery needle assembly for system WO2023241645A1 (en)

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CN202210679191.3A CN117288548A (en) 2022-06-16 2022-06-16 System and method for vaporizing a sample and a delivery needle assembly for use in the system
CN202210679191.3 2022-06-16

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US5432098A (en) * 1994-10-31 1995-07-11 Dynatech Precision Sampling Corporation Apparatus, and process, for automatically sampling solids and semi-solids materials for analysis
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